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China Anhui Wanyi Science and Technology Co., Ltd.
Anhui Wanyi Science and Technology Co., Ltd.
Anhui Wanyi Science and Technology Cooperated Limited Company founded in 2003, is a professional manufacturer and supplier of analytical instruments with an international vision and operational standards, whose leading products cover chromatography, spectroscopy, mass spectrometry and varieties of industrial applications such as environment monitoring, leak detection, industrial intelligence, industrial process, medical devices. The total number of employees is more than 1400, including 500 ...
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Determination of Sugars in Tobacco by Ion Chromatography
Determination of Sugars in Tobacco by Ion Chromatography
Determination of Sugars in Tobacco by Ion Chromatography   Water-soluble sugars mainly refer to glucose, fructose and sucrose, which are common sugars in tobacco. And they play a very important role in both the quality of tobacco and tobacco products, as well as the flavor and taste of cigarettes.   In this paper, an ion chromatography is used to determine the content of water-soluble sugar. Experimenters use IC6300 ion chromatography with an ampere detector. eluent: NaOH and sodium acetate. simple pre-treatment, with good recovery and high sensitivity, this method is suitable for the determination of water-soluble sugars.   Keywords: tobacco products; sugars; ion chromatography   1. Experiment Section   1.1 Instruments and Reagents   Wayeal IC6300 Series Ion Chromatography   Ion chromatography: Wayeal IC6300 series ion chromatography with ampere detector (Au working electrode) Auto sampler: AS2800 Sugar column: 250mm*4.0mm D-(+) Glucose, anhydrous (99%); Fructose (99%); E-(+) Sucrose, AR; Benzoic acid (99%); Disposable syringe (2mL) Water system syringe filter One ten-thousandth electronic balance Water is prepared by the ultrapure water purifier of Wayeal with a conductivity of 18.2 MΩ - cm (25 ℃).   1.2 Instrument Parameter Sugar column: 250mm*4.0mm Temperature: 30℃ Detector temperature: 35 ℃ Eluent: 250mM NaOH in A; 50mM NaOH in B; 1M sodium acetate in C; pure water in D; gradient eluting; Flow rate: 0.3mL/min Ampere detection pulse mode: Au electrode, sugars, quaternary potential Injection volume: 25uL   1.3 Sample Pretreatment Flue-cured tobacco: 0.1g sample (accurate to 0.1mg) in a 250mL conical flask, add 200mL 0.1% benzoic acid solution, put the lid on and place in an ultrasonic cell for 30min, then the solution is detected on a machine after passing through a 0.22μm filter membrane. Cigar: 0.1g sample (accurate to 0.1mg) into a 250mL conical flask, add 50mL 0.1% benzoic acid solution, put the lid on and place in an ultrasonic cell for 30min, then the solution is detected on a machine after passing through a 0.22μm filter membrane.   2. Results and Discussion   2.1 Chromatogram A series of standard working curves of 0.1mg/L, 0.5mg/L, 1.0mg/L, 2.0mg/L, 5.0mg/L, 10.0mg/L, and 20.0mg/L are pipetted respectively. Then the multipoint overlap standard curve spectra obtained according to 1.2 working conditions as shown in Figure 1. The linear correlation coefficients of glucose, sucrose and fructose under this condition are above 0.999 with good linearity.   Figure 1 Overlapping Chromatogram of Glucose, Sucrose and Fructose   Figure 2 Standard Curve of Glucose   Figure 3 Standard Curve of Sucrose   Figure 4 Standard Curve of Fructose   No Compound Linear Equation (math.) Correlation Coefficient 1 Glucose y=3044.02000x+431.15880 0.99941 2 Sucrose y=896.97000x+88.82726 0.99933 3 Fructose y=1723.92600x+174.80090 0.99941   2.2 Sample Result Cigar and flue-cured tobacco samples are detected under the working conditions of 1.2. The sample chromatogram are shown as Figures 5 and 6. The target glucose, sucrose and fructose peaks in the sample chromatogram are symmetrical with good separation and non-interfering peaks.   Figure 5 Chromatogram of Cigar   Fig. 6 Chromatogram of Flue-cured Tobacco   Table 2. Sample Results Samples compound Sample Test Content/%   Flue-cured Tobacco -1 Glucose 1.87 Sucrose 0.45 Fructose 1.73   Flue-cured Tobacco - 2 Glucose 1.93 Sucrose 0.44 Fructose 1.65   Cigar-1 Glucose 0.024 Sucrose N.D. Fructose 0.03   Cigar-2 Glucose 0.025 Sucrose N.D. Fructose 0.03     3.Conclusion   An ion chromatography method for the determination of sugar in tobacco products is established by using Wayeal 6300 series ion chromatography with an ampere detector. The samples were pre-treated and then separated by an ion chromatography column and quantified by external standard method, which is capable of qualitative and quantitative analysis of water-soluble sugars in the samples. The method is simple and easy to operate, with good repeatability, sensitivity and accuracy, which can be used for the determination of sugar content in tobacco products.
2024-09-06
Determination of Six Conventional Cations in Wine by Ion Chromatography
Determination of Six Conventional Cations in Wine by Ion Chromatography
Determination of Six Conventional Cations in Wine by Ion Chromatography     In this test, an ion chromatograph is used to test the six cations in wine. The method is simple, with good linearity and stable repeatability, and fully meets the testing requirements.   1. Experiment   1.1 Main Instruments and Reagents Ion Chromatograph: IC6600 series with conductivity detector, cation suppressor, autosampler AS3110 series. Chromatography Column: MS-5C-P2, 4.6*250mm, 5μm Guard Column: MS-5CG, 4*30mm Li+ Standard Solution (1000mg/L) Na+ Standard Solution (1000mg/L) NH4+ Standard Solution (1000mg/L) K+ Standard Solution (1000mg/L) Mg2+ Standard Solution (1000mg/L) Ca2+ Standard Solution (1000mg/L) Disposable Syringe (2mL) Aqueous Microporous Filter Membrane(0.45μm) Pretreatment Column: RP column White Wine Yellow Wine Wine   1.2 Solution Preparation 1.2.1 Mixed Standard Solution Pipette 0.1mL of Li+ standard solution (1000mg/L) into a 100mL volumetric flask, dilute and fix the volume with water, mix well; prepared to Li+ standard solution of 1.0 mg/L. Pipette 10mL of NH4+standard solution (1000mg/L), 10mL of Ca2+ standard solution (1000mg/L), 10mL of Mg2+ standard solution (1000mg/L) in one 100mL volumetric flask, dilute and fix the volume with water, mix well; prepared a standard solution containing 100mg/L of NH4+, 100mg/L of Mg2+, and 100mg/L of Ca2+ mixed standard solution.   1.2.2 Standard Working Solution Pipette 0.1mL, 0.2mL, 0.5mL, 1mL, 2 mL, 5mL, 10mL, 20mL of Li+ standard solution (1.0mg/L), 0.05mL, 0.1mL, 0.2mL, 0.5mL, 1mL, 4mL, 10mL of NH4+, Mg2+, and Ca2+ mixed standard solution (100mg/L) respectively, 0.05mL, 0.1mL, 0.2mL, 0.5mL, 0.8mL, 1mL, 1.5mL, 2.0mL of Na2+ standard solution (1000mg/L), K+ standard solution (1000mg/L) 0.01mL, 0.05mL, 0.1mL, 0.2mL, 0.5mL, 1mL, 2mL, 5mL. Put in a set of 100mL volumetric flasks, diluted and fix the volume with water, mix well, and prepared into 8 different concentrations of the mixed standard series, the standard series of mass concentration is shown in Table 1.   Table 1 Concentration Gradient Table of Standard Curve Concentration Gradient Table of Standard Curve Compounds Standard 1 Standard 2 Standard 3 Standard 4 Standard 5 Standard 6 Standard 7 Standard 8 Li+ 0.001 0.002 0.005 0.01 0.02 0.05 0.1 0.2 Na+ 0.5 1 2 5 8 10 15 20 NH4+ 0.05 0.1 0.2 0.5 1 4 10 20 K+ 0.1 0.5 1 2 5 10 20 40 Mg2+ 0.05 0.1 0.2 0.5 1 4 10 20 Ca2+ 0.05 0.1 0.2 0.5 1 4 10 20   1.3 Instrument Working Condition Chromatography Column: MS-5C-P2, 4.6*250mm, 5μm Guard Column: MS-5CG, 4*30mm Temperature: 40°C Conductivity Cell Temperature Eluent: 22mM MSA Flow Rate: 1.0mL/min Suppressor Current: 66mA Injection Volume: 25μL   1.4 Sample Pretreatment A disposable syringe is used to aspirate the sample and pass it through the pre-treatment cartridge RP column and 0.45μm aqueous filtration membrane for the removal of organic matter in the sample, and 0.45μm aqueous filtration membrane for the removal of particulate matter in the sample.   2. Result and Discussion   2.1 Separation Verification In 1.3 working conditions of the mixed standard solution, the standard chromatograms of 9 cations are shown in Fig. 1, and the test results are shown in Table 2. After testing, the peak shapes of the nine cations are symmetrical, and the separation of the components is good.   Fig 1 Chromatogram of 9 Ions Mixed Standard   Compounds Retention Time Peak Area Concentration (mg/L) Separation SNR Li+ 5.187 37.931 0.5 4.706 13499.755 Na+ 6.230 45.849 2.0 2.607 14459.840 NH4+ 6.937 57.247 2.5 2.879 13938.415 Methylamine 7.807 77.165 10 3.487 19271.353 K+ 8.917 69.240 5.0 2.122 15502.730 Dimethylamine 9.680 60.338 10 6.530 11867.878 Trimethylamine 12.990 92.716 20 9.382 10502.103 Mg2+ 20.733 103.154 2.5 5.505 7213.676 Ca2+ 27.818 121.626 5.0 n.a. 5695.913 Table 2 Testing Result of 9 Ions Mixed Standard   2.2 Verification of Standard Curve Linearity The working solution of the standard curve series prepared in 1.2.2 was injected into the system and analyzed according to the working conditions of 1.3, and the linearity of the standard curve was obtained as shown in Table 3 below, with good linearity.   Table 3 Linearity of Standard Curve Compounds Curvilinear Equation Correlation Coefficient R Li+ y=72.29391x-0.08781 0.99986 Na+ y=19.99226x+0.47697 0.99994 NH4+ y=0.25375x2+16.16416x+1.42735 0.99999 K+ y=13.36620x-0.31093 0.99999 Mg2+ y=37.96758x-2.36348 0.99996 Ca2+ y=23.39661x-1.85857 0.99986   2.3 Sample Testing Samples of white wine, yellow wine and wine are tested according to 1.4 Sample pretreatment method, and the test spectra are shown in Fig. 3, Fig. 4 and Fig. 5, and the data are shown in Table 4 below.   Fig 3 White Wine Chromatogram of 6 Repeated Injections   Fig 4 6 Repeated Injections Chromatogram of Wine Diluted 20 Times   Fig 5 6 Repeated Injections Chromatogram of Yellow Wine Diluted 20 Times   Table 4 Test Data Sample Li+(mg/L) Na+(mg/L) NH4+(mg/L) K+(mg/L) Mg2+(mg/L) Ca2+(mg/L) White Wine 0.0019 2.44 0.576 0.128 0.191 0.627 Yellow Wine 0.0108 32.123 150.703 281.49 74.55 114.137 Wine 0.0097 43.727 11.314 694.748 51.575 47.377   Note: The relative standard deviations (RSDs) of the retention times and peak areas of the six cations were from 0.014% to 0.063% and 0.223% to 1.415%, respectively, and the spiked recoveries were in the range of 84.5%~108%.   3. Conclusion The ion chromatography for the determination of six cations in wine shows good separation, good linearity, stable repeatability and high sensitivity. It can fully meet the requirements for the testing of the six cations in wine.              
2024-09-11
Troubleshooting of High Performance Liquid Chromatography (HPLC)
Troubleshooting of High Performance Liquid Chromatography (HPLC)
Troubleshooting of High Performance Liquid Chromatography (HPLC)   There are many test instruments used in the laboratory, and high-performance liquid chromatography (HPLC) is one of them. The instrument is based on classical chromatography, citing the theory of gas chromatography, and technically it changes the traditional mobile phase to high-pressure delivery. This article will give you the brief introduction of the chromatography, characteristics, failure causes, and treatment methods of high-performance liquid chromatography (HPLC).     Introduction of High-performance Liquid Chromatography   High performance liquid chromatograph (HPLC) is an instrument based on the principle of high performance liquid chromatography, which is mainly used to analyze less-volatile and thermal-unstable organic compounds with high boiling point and large molecular weight. It consists of solvent bottles, pump, sample injector, chromatographic column, detector, recorder and workstation.     How does high performance liquid chromatography work?   The mobile phase in the reservoir is pumped into the system by a high-pressure pump, and the sample solution passes through a sample injector then enters the mobile phase, which loads the sample solution into a chromatographic column (stationary phase). Because the various components in the sample solution have different distribution coefficients in the two phases, when they are moving relatively in the two phases, after repeated adsorption-desorption distribution processes, the moving speed of each component is greatly different, and the components are separated into single components flowing out of the column in turn. When passing through the detector, the sample concentration is converted into electrical signal and transmitted to the recorder, and the data is printed out in the form of chromatogram.     Applications of High-Performance Liquid Chromatography   HPLC is widely used in food, pharmaceutical, environment, agriculture and scientific research   1. Application in environmental analysis: It can be used for the analysis of cyclic aromatic hydrocarbons (PAHs), pesticide residues, etc.   2. Application in food analysis: It can be used for food nutrition analysis, food additive analysis, food contaminant analysis, etc.   3. Application in life science: Purification, separation, and determination of molecular weight substances in life science, genetic engineering, clinical chemistry, molecular biology, and biochemistry can be studied at the molecular level.   4. Application in the medical examination: analysis and determination of metabolites in body fluids, pharmacokinetics, clinical drug monitoring, etc.   5. Application in inorganic analysis: analysis of anions and cations, etc.     Common Faults and Treatment Methods of High-Performance Liquid Chromatography   Fault Description Cause Analysis Solution   Front panel status indicator does not light up Cable connection failure Open the chassis and reconnect reliably Switching power supply module cannot work and supply power Replace the switching power module Signal intensity too low Bubbles are generated in the flow cell Flush the flow cell and degasify the mobile phase   Prompt deuterium lamp failure Deuterium lamp cannot be lit Restart the instrument. If the fault cannot be eliminated, please replace the deuterium lamp.     Common troubleshooting of autosampler   Fault Description Cause Analysis Solution Abnormal electrical initialization of the instrument­­­ Software prompts: The zero-point optocoupler of the horizontal motor fails. 1.  Restart the instrument 2.  Check the sample chamber for any obstacles 3.  Check the sensor at the corresponding position for any obvious abnormal phenomena such as looseness and line breakage 4.  Call the after-sale service to solve the problem Software prompts: The zero-point optocoupler of the vertical motor fails. Software prompts: The zero-point optocoupler of the tray motor fails. Software prompts: The zero-point optocoupler of the syringe motor fails. Software prompts: EEPROM is unable to read or write. 1.  Restart the instrument 2.  Call the after-sale service to solve the problem The software for the injection process indicated an exception Software prompts: Sample vial is missing 1.  Check whether the sample vial position is consistent with the software setting position 2.  Restart the instrument 3.  Call the after-sale service to solve the problem Software prompts: The door is open 1.  Check whether the door is normally closed 2.  Check the door sensor for abnormalities 3.  Restart the instrument 4.  Call the after-sale service to solve the problem Line fault The status light on the front panel is not on 1.  Restart the instrument 2.  Check whether the power cord is reliably connected 3.  Check whether the power switch is on 4.  Check the fuse for damage 5.  Call the after-sale service to solve the problem The autosampler does not trigger the chromatogram 1.  Check whether the trigger line is reliably connected 2.  Check whether the instrument serial line is connected reliably 3.  Check whether the software instrument networking light is flashing Fluid line fault There are obvious bubbles in the syringe during injection 1.  Perform flushing fluid line process 2.  Check whether the pipe joints are loose 3.  Check joints for leakage 4.  Too little liquid in the sample vial There are small bubbles in the fluid line during injection Poor reproducibility of sample injection 1.  No ultrasonic processing to the sample 2.  No ultrasonic processing to the wash solvent 3.  There are obvious air bubbles in the pipeline syringe during injection 4.  The sample vial was reused without cleaning   Common troubleshooting of pump   Fault Description Cause Analysis Solution If the front panel status indicator is not light, the connection may be loose, Open the shell, and reconnect reliably. Detection of power supply module Replacement power supply module Pump pressure is 0 pump head with air Open purge valve, with syringe pumping, until there is liquid from the empty valve flow, and then tighten the valve. Pressure alarm pressure limit range setting unreasonable According to the actual test needs, set a reasonable pressure limit range. Pipeline blockage leads to excessive pressure. Check whether the pipeline is gambling after pump head. Leakage causes too little pressure Check whether there is any damage to all levels of pipelines and streets after the pump head. The buzzer keeps buzzing at a frequency of 0.5HZ. Motor blocked, pressure upper limit alarm, pressure lower limit alarm, liquid leakage alarm. Check and determine the cause of the error, and then solve it according to the situation The buzzer beeps 3 times at a frequency of 1HZ and then stops Leak sensor failure, pressure sensor failure, fan failure, photoelectric switch failure, solvent threshold alarm, unsuccessful initialization. Check and determine the cause of the error, and then solve it according to the situation                        
2022-08-24
Determination of Cadmium in Food by Atomic Absorption Graphite Furnace Method
Determination of Cadmium in Food by Atomic Absorption Graphite Furnace Method
Determination of Cadmium in Food by Atomic Absorption Graphite Furnace Method   This paper establishes an analytical method for the determination of cadmium in food by atomic absorption graphite furnace method with reference to the standard “GB 5009.15-2023 National Standard for Food Safety Determination of Cadmium in Food”.   Keywords: Atomic absorption, autosampler, food, cadmium   1. Experiment Method   1.1 Instrument Configuration Atomic Absorption Spectrophotometer AA2300 Series   Table 1 Configuration List of Atomic Absorption Spectrophotometer No Modular Qty 1 Atomic Absorption Spectrophotometer AA2310 1 2 Graphite Furnace 1 3 Autosampler 1 4 Cooling Water Circulator 1 5 High Purity Argon 1 6 Graphite Tube 1   1.2 Reagents and Experiment Material 1.2.1 Nitric acid solution (1+99):Pipette 10mL of nitric acid and slowly add to 990mL of water and mix well. 1.2.2 Cd Standard Solutions: 100mg/L 1.2.3 One in ten thousand analytical balances 1.2.4 Centrifuge   1.3 Sample Pretreatment Take 0.05g sample or more (between 0.05~0.0.08), and add 10mL of 3% dilute nitric acid to the sample. Shake for 5min and centrifuge at 8000r/min for 12min. Take the supernatant and test on the machine.   2. Result and Discussion   2.1 Spectral Conditions of Cadmium   Heating Method Graphite Furnace Method Testing Method Peak Height Injection Volume 20μL Spectral Bandwidth 0.4nm Characteristic Wavelength 228.8nm Ignite Method AA-BG Lamp Current 3mA   2.2 Standard Curve Testing and Sample Chromatogram   Gradient Concentration Table of Standard Curve(ng/mL) Curve Point 1 2 3 4 Cadmium standard solution 0.40 1.20 1.60 2.00   2.3 Linearity of Standard Curve   3. Conclusion   From the experimental results, the linear correlation coefficient of cadmium in the concentration range of 0.40-2.00ng/mL is greater than 0.999. The method is accurate, reliable and sensitive, and can be used for the determination of cadmium in food.                                
2024-09-06
Determination of Sugar Alcohol in Food by High Performance Liquid Chromatography
Determination of Sugar Alcohol in Food by High Performance Liquid Chromatography
Determination of Sugar Alcohol in Food by High Performance Liquid Chromatography     1. Method and Principle   Determined by high performance liquid chromatography with an RID detector and quantified by external standard method.   2. Instrument Configuration and Experimental Methods   2.1 Instrument Configuration No. System Configurations Qty 1 P3210B Binary High Pressure Gradient Pump 1 2 CT3210 Colum Oven 1 3 AS3210 Autosampler 1 4 RI Detector 1 5 4.6*250mm 5μm Amino Column 1 6 SmartLab Workstation 1   Table1 Configuration List 2.2 Experimental Method 2.2.1 Preparation of Reagents and Standards No. Reagents Purity 1 Acetonitrile Chromatographically pure 2 4 kinds of sweeteners mix standards 40g/L Table 2 List of Reagents and Standards   Standard curve: The mixed standard (40 mg/mL) of the four sweeteners was diluted with water to a concentration of 1.6 mg/mL, 2.4 mg/mL, 3.2 mg/mL, 4.0 mg/mL, 4.8 mg/mL , 6.0 mg/mL series of concentration working curves.   2.22 Chromatography Conditions Chromatography Column Amino column, 4.6*250mm, 5μm Mobile Phase Acetonitrile :Water=80:20 Flow Rate 1mL/min Temperature 30°C Cell Temperature 40°C Injection Volume 20μL Table 3 Chromatography Conditions 2.2.3 Sample Pretreatment Samples of non-protein beverages should not be less than 200 mL and placed in an airtight container after being fully mixed. 10g of sample into a 50 mL volumetric flask, and fix the volume to 50 mL with water, shake well and detected on a machine after passing through a 0.22μm filter membrane.   3. Experimental Results   3.1 System Suitability   Figure 1 Chromatogram of 6.0mg/mLsweetener mixing standard   Notes: As the figure shows, there are good shape peaks of erythritol, xylitol, sorbitol and maltitol, and no other peaks around the target peaks, which meet the experimental requirements.   3.2 Linearity Figure 2 Standard Curve of Erythritol   Figure 3 Standard Curve of Xylitol   Figure 4 Standard Curve of Sorbitol                                         Figure 5 Standard Curve of Maltose   The concentrations of mixing standard curves of the four sweeteners are 1.6 mg/mL, 2.4 mg/mL, 3.2 mg/mL, 4.0 mg/mL, 4.8 mg/mL, and 6.0 mg/mL. As the figure shows, the linear correlation coefficients of the standard curves of four sweeteners are above 0.999, which satisfied the experimental requirements.   3.3 Repeatability   Figure 6 Repeatability Chromatogram of 6 Injections of 3.2mg/mL Sweetener Mixing Standard         Retention Time No. Erythritol Xylitol Sorbitol Maltitol 1 8.407 11.365 15.637 36.644 2 8.414 11.374 15.638 36.658 3 8.415 11.377 15.644 36.645 4 8.412 11.374 15.638 36.635 5 8.426 11.391 15.670 36.696 6 8.436 11.405 15.680 36.701 RSD(%) 0.128 0.128 0.120 0.077 Table 4 6 Injections of Retention Time Repeatability         Peak Area No. Erythritol Xylitol Sorbitol Maltitol 1 228.976 239.243 234.601 224.837 2 230.029 238.083 239.130 224.900 3 224.656 237.784 236.914 222.373 4 227.415 239.595 238.192 222.414 5 227.455 240.591 238.963 223.679 6 228.492 239.876 237.412 227.865 RSD(%) 0.809 0.450 0.705 0.913 Table 5 6 Injections of Peak Area Repeatability   Note: As the table shows, the retention time RSD of erythritol, xylitol, sorbitol and maltitol are 0.128%, 0.128%, 0.120%, 0.077%, and the repeatability of retention time was less than 0.2%, which satisfied the experimental requirements. The peak area RSDs of erythritol, xylitol, sorbitol and maltitol are 0.809%, 0.450%, 0.705% and 0.913%. The repeatability of peak area was less than 1%, which satisfied the experimental requirements.   3.4 Detection Limit   Figure 7 Chromatogram of 1.6mg/mL Sweetener Mixing Standard   Note: As the Figure 7 shows, the concentration of 1.6 mg/mL sweetener mixing standard, the triple SNR is calculated from the detection limits of erythritol, xylitol, sorbitol, and maltitol are 0.01 mg/mL, 0.012 mg/mL, 0.015 mg/mL, and 0.03 mg/mL, which meet the experimental requirements.   3.5 A branded Non-protein Beverage   Figure 8 Chromatogram of a Branded Beverage in 2 Injections   Samples Peak Area Sample-1 209.594 Sample-2 209.001 Arithmetic Mean Value 209.298 Table 6 2 Injections for a Branded Beverage   As the chromatogram shows, erythritol is detected in a branded beverage and xylitol, sorbitol and maltitol are not detected. The test results are consistent with the ingredient list. The data in the table are the results of two tests with an absolute difference of 0.14% of the arithmetic mean, which is less than 10% of the standard requirement.   3.6 Attentions   Since the differential refractive index detector is sensitive to the density of the solution, it is recommended that the mobile phase be premixed when doing the experiment.   4 Conclusion   The analytical method introduced in this article refers to the national standard GB 5009.279-2016 (Determination of xylitol, sorbitol, maltitol and erythritol in food), by using a Wayeal LC3200 series high performance liquid chromatograph with a RID detector. The experimental results showed that the system adaptive testing of erythritol, xylitol, sorbitol and maltitol, the peaks are good and there are no other peaks around the target peaks. The RSDs for retention time are 0.128%, 0.128%, 0.120%, and 0.077%, all less than 0.2%. The RSDs of peak area are 0.809%, 0.450%, 0.705%, 0.913% and less than 1%. SNR=3 as detection limit, then detection limits of erythritol, xylitol, sorbitol, and maltitol are 0.01 mg/mL, 0.012 mg/mL, 0.015 mg/mL, and 0.03 mg/mL. The absolute difference between the two measurements is 0.14% of the arithmetic mean, which is less than 10% of the standard requirement. All the above data shows that the results satisfy the experimental requirements.              
2024-09-05
Determination of Tyrosol in Wine by High Performance Liquid Chromatography
Determination of Tyrosol in Wine by High Performance Liquid Chromatography
Determination of Tyrosol in Wine by High Performance Liquid Chromatography   1. Instrument Configuration and Experiment Methods   1.1 Instrument Configuration   Table 1 Configuration List of Liquid Chromatography No Module Qty 1 P3210B Binary Pump System 1 2 CT3400 Column Oven 1 3 AS3210 Autosampler 1 4 UV 3210 UV Detector 1 5 C18 Column, 4.6*250mm 5μm 1 6 SmartLab Workstation 1   1.2 Experiment Method   1.2.1 Reagent Preparation No Reagents Purity 1 Methanol Chromatographic Grade 2 Tyrosol Standard 98%   1.2.1.1 Tyrosol standard stock solution (1000mg/L): Take the appropriate amount of tyrosol standard, dissolve and Fix the volume with methanol, a standard stock solution with a concentration of 1000mg/L will be prepared, sealed and stocked at -4℃.   1.2.1.2 Tyrosol standard working solution: Pipette the appropriate amount of tyrosol standard stock solution accurately, dilute with methanol to form a series of working curves with concentrations of 0.1mg/L, 1mg/L, 1.5mg/L, 3mg/L, 5mg/L, 7.5mg/L, 10mg/L respectively.   1.2.2 Chromatography Conditions   Table 3 Chromatography Conditions Chromatography Column C18 Column 4.6*150mm, 5μm Mobile Phase A: Methanol, B: Water Flow Rate 1mL/min Column Temperature 40°C Wavelength 222nm Injection Volume 10μL   Table 4 Proportion of Mobile Phase Time/min A B 0 30 70 9 35 65 9.1 100 0 12 100 0 13 30 70 20 30 70   1.2.3 Sample Pretreatment   Take appropriate amount of white wine samples, through the 0.45μm microporous filter membrane, then to be measured.   2. Experimental Result   2.1 System Suitability Fig 1 Chromatogram of 10mg/L Standard   Table 5 10mg/L Standard Test Data Compounds Retention Time Peak Height Peak Area Theoretical Plate Number Tyrosol 7.209 29.398 367.785 7558     Note: From the chromatogram and data, it can be seen that the tyrosol peak shape is good, there are no other peaks around the target peak, and the theoretical plate number is high, which meets the experimental requirements.   2.2 Standard Curve                                        Fig 2 Test Result of Standard Curve   Note: From the above chromatogram, it can be seen that the correlation coefficient value R of tyrosol curve is above 0.999, which meets the experimental requirements.   2.3 Repeatability   Fig 3 Repeatability Chromatogram of 3.75mg/L Standard for 6 Injections   Table 6 Repeatability Test Data of 6 injections for 7.5mg/L Standard         Tyrosol No. Retention Time Peak Area 1 7.205 284.108 2 7.209 286.256 3 7.210 285.346 4 7.216 285.676 5 7.212 286.806 6 7.207 288.199 RSD (%) 0.053 0.485   Note: According to the above table data, it can be seen that the RSD of tyrosol retention time repeatability is 0.053% and the RSD of peak area repeatability is 0.485%, both of which has good repeatability. It meets the experimental requirements.   2.4 Detection Limit Fig 4 Test Chromatogram of 0.1mg/L Standard                                         Table 7 Test Data of 0.1mg/L Standard Compound Retention Time Peak Area SNR Tyrosol 7.210 4.852 41.562   Note: According to the above table data, the detection limit of tyrosol is 0.0073mg/L with 3 times signal-to-noise ratio, which meets the experimental requirements.   2.5 Test Results of a Brand of White Wine Fig 5 Test Chromatogram of a Brand White Wine   Table 8 Test Data of a Brand White Wine Compound Retention Time Peak Area Sample Volume Tyrosol 7.210 4.852 0.275mg/L   Note: 0.275 mg/L of tyrosol was detected in a brand of white wine.   2.6 Spiked Testing Result of a Brand White Wine Fig 6 Spiked Testing Chromatogram of a Brand White Wine   Table 9 Spiked Test Data of a Brand White Wine Compounds Retention Time Peak Area Sample Volume Tyrosol 7.234 71.425 1.799mg/L   Note: Add 15μL of 100mg/L standard in a 1mL white wine, and according to the detection concentration of white wine and the spiked concentration, the theoretical concentration is 1.775 mg/L. From the detection concentration in the above table, the spiked recovery is 101.4%, which meets the experimental requirements.   2.7 Attentions The Tyrosol Standard stock solution needs to be stored at low temperature, otherwise its content will decrease.     3. Conclusion This article introduces the determination of tyrosol content in white wine by Wayeal high performance liquid chromatograph LC3210 series equipped with ultraviolet detector. The experimental results showed that the peak shape of tyrosol is good in the system adaptability test, and there are no other peaks around the target peak, and the theoretical plate number is high, which met the experimental requirements. The curve correlation coefficient R value is above 0.999. The RSD of tyrosol retention time is 0.053%, and the RSD of peak area is 0.485%, which is good reproducibility. The detection limit of tyrosol is 0.0073mg/L. The recoveries are 101.4% with the spiked 1.5mg/L in the sample. The results of the above data meet the requirements of the instrument for the test method.                        
2024-09-05
Determination the Content of Acyclovir by High Performance Liquid Chromatography
Determination the Content of Acyclovir by High Performance Liquid Chromatography
Determination the Content of Acyclovir by High Performance Liquid Chromatography   The analytical method introduced in this article, with reference to the 2020 edition of the Pharmacopoeia of the People's Republic of China in Acyclovir test method, by using Wayeal high performance liquid chromatograph LC3200 series with a DAD detector.   1. Instrument Configuration and Experiment Method   1.1 Instrument Configuration No Name Qty 1 P3210Q Quaternary Pump 1 2 CT3400 Column Oven 1 3 AS3210 Autosampler 1 4 DAD3260 DAD Detector 1 5 Nova Atom PC18 4.6x250mm 5μm 1 6 Chromatography Workstation 1   1.2 Experiment Method   1.2.1 Reagents Preparation   Table 2 List of Reagents No Reagents Purity 1 2 3 4 5 Methanol Phosphoric acid Sodium hydroxide Acyclovir Guanine Chromatographic Purity(LC) GR MOS 98% 99%   1.2.1.1 Test solution: Take 40mg of sample into a 200mL measuring flask, add 2mL of 0.4% sodium hydroxide to dissolve it, then add 25mL of 0.1% (V/V) phosphoric acid solution and dilute it with water to the scale, shake well.   1.2.1.2 Reference solution: Take 1mL of the test solution into a 100mL measuring flask, add 5mL of 0.1% phosphoric acid solution, dilute with water to scale and shake well.   1.2.1.3 Guanine control storage solution: Take 10mg of guanine reference into a 50mL measuring flask, add 5mL of 0.4% sodium hydroxide solution to dissolve it, then add 5mL of 0.1% phosphoric acid solution, dilute it with water to the scale, shake well.   1.2.1.4 Guanine reference solution: Take 1mL of guanine reference storage solution into a 100mL flask, dilute with water and shake well.   1.2.1.5 System suitability solution: Take appropriate amount of each of the reference solution and guanine reference solution, mix in equal volume and shake well.   1.2.2 Chromatography Condition   Table 3 Chromatography Conditions Chromatography Column Nova Atom PC18 Chromatography Column, 4.6*250mm, 5μm Mobile Phase Mobile Phase A: Water Mobile Phase B: Methanol Flow Rate 1mL/min Column Temperature 35°C Wavelength 254nm Injection Volume 20μL   Table 4 Mobile Phase Ratio Time (min) Mobile Phase A Mobile Phase B 0 94 6 15 94 6 40 65 35 41 94 6 51 94 6   2. Experiment Result   2.1 System Suitability Solution Fig 1 Test Chromatogram of System Suitability Solution   Table 5 Test Data System Suitability Solution No Compound Retention Time Peak Area Theoretical plate number Separation 1 Guanine 5.698 138.675 17173 12.334 2 Acyclovir 8.425 139.902 15786 n.a.   Note: From the above graph and the data in the table, it can be seen that Acyclovir and Guanine have better peak shapes and high theoretical plate number. The degree of separation is more than 3.0, which meets the requirements in pharmacopoeia.   2.2 Repeatability Fig 2 Repeatability Chromatogram of 6 Injections of System Suitability   Table 6 Repeatability Data of 6 Injections of System Suitability Solution Retention Time Sample No Guanine Acyclovir       Retention Time 1 5.698 8.408 2 5.701 8.415 3 5.705 8.411 4 5.701 8.405 5 5.705 8.401 6 5.705 8.398 RSD (%) 0.048 0.074     Table 7 Repeatability Data of 6 Injections of System Suitability Solution Peak Area Sample No Guanine Acyclovir       Peak Area 1 136.997 138.836 2 138.496 139.117 3 137.783 139.505 4 136.663 138.204 5 137.755 137.968 6 137.789 139.374 RSD (%) 0.475 0.452   Note: According to the data in the above table, the RSD of retention time of guanine and acyclovir in the system suitability solution is 0.048% and 0.074%, and the RSD of peak area is 0.475% and 0.452%, respectively. The reproducibility results are good and meet the experimental requirements.
2024-09-05
Application of Ion Chromatography in Environmental Analysis
Application of Ion Chromatography in Environmental Analysis
Application of Ion Chromatography in Environmental Analysis   Application of Ion Chromtography in Environmental Water Quality   With the development of social economy, water pollution has become an increasingly serious problem. In order to protect the environment and prevent water pollution, it is necessary to monitor rivers, lakes, seas and groundwater. For the treatment, recycling, comprehensive use and discharge of industrial and domestic wastewater, water quality analysis is required first. In the process of analysis, ion chromatography can be applied. The ion chromatography is widely used in water quality analysis because of its high efficiency, stability and accuracy.       Water Quality——Inorganic Anion Analysis
2024-09-05
Determination of Polyethylene Glycol by Gel Permeation Chromatography
Determination of Polyethylene Glycol by Gel Permeation Chromatography
Determination of Polyethylene Glycol by Gel Permeation Chromatography   1. Introduction   Purpose: Determination of molecular weight and distribution of polyethylene glycol (PEG) by high performance gel permeation chromatography (GPC) method.   Method: Xtimate SEC-120, 5 μm, 7.8x300 mm gel permeation chromatography column Differential refractive index detector (RID) Mobile phase: ultrapure water Flow rate: 1.0ml/min Column temperature: 35 ℃; Injection volume: 10μl. Calibration curves are established and the molecular weight and distribution results of each sample are calculated by GPC software.   Result: The linearity of PEG is good when the molecular weight was in the range of 400-20000. The reproducibility of the experiment is good, with 6 consecutive injections of PEG6000, the RSD value of retention time is 0.105%, and the RSD value of peak area is 0.335%.   Conclusion: High performance gel permeation chromatography (GPC) is a reliable method for the determination of molecular weight and distribution of PEG, which has the advantages of accurate and high reproducibility when used to evaluate the polydispersity property of polymer compounds.   Keywords: HPLC, GPC, RID, Polymer, Polyethylene Glycol   2. Experiment Method 2.1 Instrument Configuration Table 1 Configuration List of High Performance Liquid Chromatograph No Modular Qty 1 High Performance Liquid Chromatography LC3200 Series 1 2 PB3200 Binary Pump 1 3 RID3300 1 4 CT3200 Column Oven 1 5 AS3200 Autosampler 1 2.2 Test Conditions Chromatography Column: Xtimate SEC-120,5μm,7.8x300mm Column Temperature: 35°C Detector: RID Flow Rate: 1.0mL/min Mobile Phase: Water Injection Volume: 10μL   2.3 Instrument/Reagents and Consumables Reagents: Ultrapure Water Standard: PEG400; PEG2000; PEG6000; PEG10000; PEG20000 Auxiliary Equipment Analytical Balances Solvent Extraction Unit Ultrasonic Cleaner Experimental Materials Filter Membrane: aqueous filter membrane 0.45μm   2.4 Preparation of PEG Standard Pipette 0.20g each of PEG400, PEG2000, PEG6000, PEG10000 and PEG20000 standards, add 10mL of water to dissolve, mix well, and prepared the concentration of 20mg/mL samples to be tested.   3. Result and Discussion 3.1 Different Molecular Weight Standards Fig 1 Chromatogram of PEG400 Table 1 Chromatographic Parameters of PEG400 No Compounds Retention Time Peak Area Theriacal Plate Number Trailing Factor 1 PEG400 10.315 501.732 2346 1.185   Fig 2 Chromatogram of PEG2000 Table 2 Chromatographic Parameters of PEG2000 No Compounds Retention Time Peak Area Theoretical Plate Number Trailing Factor 1 PEG2000 8.659 499.892 1926 1.230   Fig 3 Chromatogram of PEG6000 Table 3 Chromatographic Parameters of PEG6000 No Compounds Retention Time Peak Area Theoretical Plate Number Trailing Factor 1 PEG6000 7.215 499.482   1.171   Fig 4 Chromatogram of PEG10000 Table 4 Chromatographic Parameters of PEG10000 No Compounds Retention Time Peak Area Theoretical Plate Number Trailing Factor 1 PEG10000 6.612 483.657 2550 1.265   Fig 5 Chromatogram of PEG20000 Table 5 Chromatographic Parameters of PEG20000 No Compounds Retention Time Peak Area Theoretical Plate Number Trailing Factor 1 PEG20000 6.081 497.803 1103 1.799   Fig 6 Overlap Chromatograms of Different Molecular Weight Note: The above data shows that the retention time of PEG20000 is 6.081 minutes, and PEG400 is 10.315 minutes, larger molecules are eluted first and smaller molecules are eluted later.   3.2 Repeatability Fig 7 Repeatability Overlap Chromatograms of PEG6000 (n=6) Table 7 Repeatability Chromatographic Parameters of PEG6000 (n=6) No Samples Retention Time Peak Area 1 6000 7.233 498.821 2 6000 7.234 503.367 3 6000 7.225 499.891 4 6000 7.221 499.560 5 6000 7.219 501.374 6 6000 7.215 499.482 Average - 7.225 500.416 RSD(%) - 0.105 0.335 Note: The repeatability is good. The RSD of retention time is 0.105% and the RSD of peak area is 0.335% for 6 injections of PEG6000.   3.3 Standard Curves Fig 8 Standard Curves Chromatograms of Different Molecular Weights Table 8 Standard Curves Chromatographic Parameters of Different Molecular Weights Note: The molecular weight and distribution results of each sample are calculated by GPC software. The linearity of PEGmolecular weight is good in the eange of 400 to 20,000, and the linear correlation coefficient is 0.999.   4. Conclusion This polyethylene glycol (PEG) test is performed by gel chromatography by using an LC3200 series high performance liquid chromatograph with differential refractive index detector. the retention time of PEG20000 is 6.081 minutes, and PEG400 is 10.315 minutes, larger molecules are eluted first and smaller molecules are eluted later. The repeatability is good. The RSD of retention time is 0.105% and the RSD of peak area is 0.335% for 6 injections of PEG6000. The linearity of PEG molecular weight is good in the range of 400 to 20,000, and the linear correlation coefficient is 0.9999. High performance gel permeation chromatography (GPC) is a reliable method for the determination of molecular weight and distribution of PEG, which has the advantages of accurate and reproducible results when used to evaluate the polydispersity property of polymer compounds.   Note: The sample should be left at room temperature for more than 12h and should be mixed gently, do not ultrasonic or shake vigorously to accelerate dissolution.    
2024-09-27
ARABLAB 2024, Dubai World Trade Centre
ARABLAB 2024, Dubai World Trade Centre
  Wayeal at ARAB LAB 2024, we are waiting for your coming!!!   24~26 September, 2024 Booth No. 933, Hall S1 Dubai World Trade Centre  
2024-09-23
Determination of Heavy Metals in Waste Resin Powder by Wayeal Atomic Absorption Spectrophotometer
Determination of Heavy Metals in Waste Resin Powder by Wayeal Atomic Absorption Spectrophotometer
  Determination of Heavy Metals in Waste Resin Powder by Wayeal Atomic Absorption Spectrophotometer   In this paper, with reference to the standard of "HJ 749-2015 Determination of Total Chromium in Solid Waste Flame Atomic Absorption Spectrophotometry" "HJ 786-2016 Determination of Lead, Zinc and Cadmium in Solid Waste Flame Atomic Absorption Spectrophotometry", an analytical method was established for the determination of the content of heavy metal elements in waste resin powder by flame atomic absorption method.   Keywords: Atomic Absorption Spectrophotometer; flame, waste resin powder; lead; cadmium; chromium.   1. Experiment Method 1.1 Instrument Configuration Table 1 Configuration List of Atomic Absorption Spectrophotometer No Name Qty 1 Atomic Absorption Spectrophotometer AA2310 1 2 Air Compressor 1 3 High-purity Acetylene 1 4 Lead Hollow Cathode Lamp 1 5 Cadmium Hollow Cathode Lamp 1 6 Chromium Hollow Cathode Lamp 1   1.2 Reagents and Instruments 1.2.1 Lead Standard Solution(1000μg/ml) 1.2.2 Cadmium Standard Solution(1000μg/ml) 1.2.3 Chromium Standard Solution(1000μg/ml) 1.2.4 Ammonium Chloride: AR 1.2.5 Nitric Acid: GR 1.2.6 Hydrochloric Acid: GR 1.2.7 Hydrofluoric Acid: GR 1.2.8 Perchloric Acid: GR 1.2.9 30% Hydrogen Peroxide: GR 1.2.10 One in ten thousand analytical balances 1.2.11 Digital display electric hot plate   1.3 Pre-processing 1.3.1 Pre-processing of Lead and Cadmium Samples Take 0.2g of sample (accurate to 0.1mg) into a 50ml PTFE crucible. After wetting with water, 5ml of hydrochloric acid was added and the sample was heated on a hot plate in a fume hood at about 120 ℃ to initially disintegrate the sample, and then removed and cooled slightly after evaporation until about 3m remained. Add 8ml of nitric acid, 8ml of hydrofluoric acid and 4ml of perchloric acid, cover and heat at about 160 ℃ on a hot plate for 3h. Open the lid, the electric heating plate temperature control at 180 ℃ to continue heating, and often shake the crucible. When heated to a thick white smoke, cover to fully decompose the black organic carbons. After the black organic matter on the crucible wall disappears, open the lid, drive away the white smoke and steam until the contents are viscous. Take down the crucible, slightly cold, add 0.2mL nitric acid to dissolve the soluble residue, after cooling, transfer the whole amount to 50ml volumetric flask, rinse the crucible lid and inner wall with appropriate amount of experimental water, the washing solution was incorporated into 50ml volumetric flask, and the fix the volume with experimental water, shaken well, and then left to be measure. If there are undissolved particles in the digested solution, filtering and centrifugation or natural precipitation are required. (Note: Do not allow a lot of bubbles to come out when heating, otherwise it will cause loss of the sample.)   1.3.2 Pre-processing of Chromium Sample Take 0.2g (accurate to 0.0001g) of sample into a 50ml PTFE crucible. After wetting with water, 10ml of concentrated hydrochloric acid was added and the sample was heated on a hot plate in a fume hood at 50°C to initially decompose the sample. When evaporated to about 3ml, add 5ml of concentrated nitric acid, 5ml of hydrofluoric acid, cover and heat on the hot plate at about 120~130 ℃ for 0.5~1h, then open the lid, drive away the white smoke and steam until the contents are in the form of liquid beads in a non-flowing state (observe while hot). Depending on the condition of digestion, add 3ml of concentrated nitric acid, 3ml of hydrofluoric acid, 1ml of hydrogen peroxide, and repeat the above digestion process. Take down the crucible, slightly cold, add 0.2mL nitric acid to dissolve the soluble residue, transfer all the test solutions to a 50ml volumetric flask, add 5ml of 110% ammonium chloride solution, and fix the volume with experimental water, left to be measured. (Note: the total amount of 30% hydrogen peroxide added shall not exceed 10ml.)   2. Results and Discussion Lead Detection Sample Lead Burner Hight 10mm Acetylene Flow Rate 2.0L/min Spectral Bandwidth 0.4nm Wavelength 283.3nm Lighting Way AA Lamp Current 5mA   Gradient Concentration Table (mg/L) of Lead Standard Curves and Sample Data Concentration Level 1 2 3 4 5 6 Concentration of Standard Solutions (mg/L) 0.5 1.0 2.0 4.0 8.0 10 Absorbance of Standard Solutions (abs) 0.0073 0.0136 0.0290 0.0578 0.1112 0.1353 Absorbance of Waste Resin Powder (abs) 0.0024 Concentration of Waste Resin Powder (mg/L) 0.0000 Lead Concentration of Waste Resin Powder (mg/kg) Not Detected   Standard Curve of Lead Cadmium Detection Sample Cadmium Burner Height 10mm Acetylene Flow Rate 2.0L/min Spectral Bandwidth 0.4nm Wavelength 228.8nm Lighting Way AA Lamp Current 3mA   Gradient Concentration Table (mg/L) of Cadmium Standard Curve and Sample Data Concentration Level 1 2 3 4 5 Concentration of Standard Solutions (mg/L) 0.2 0.4 0.6 0.8 1.0 Absorbance of Standard Solutions (abs) 0.0667 0.0124 0.1775 0.2280 0.2748 Absorbance of Waste Resin Powder (abs) 0.0057 Concentration of Waste Resin Powder (mg/L) 0.0000 Cadmium Centration of Waste Resin Powder (mg/kg) Not Detected   Standard Curve of Cadmium Chromium Detection Sample Chromium Burner Height 10mm Acetylene Flow Rate 3.6L/min Spectral Bandwidth 0.2nm Wavelength 357.9nm Lighting Way AA Lamp Current 5mA   Gradient Concentration Table (mg/L) of Chromium Standard Curve and Sample Data Concentration Level 1 2 3 4 5 Concentration of Standard Solutions (mg/L) 0.2 0.4 0.6 0.8 1.0 Absorbance of Standard Solutions (abs) 0.0175 0.0388 0.0588 0.0786 0.0994 Absorbance of Waste Resin Powder (abs) 0.0130 Concentration of Waste Resin Powder (mg/L) 0.1519 Chromium Concentration of Waste Resin Powder (mg/kg) 37.7   Standard Curve of Chromium 3. Notes 3.1 Nitric acid and perchloric acid used in the experiment have strong oxidizing and corrosive properties, hydrochloric acid and hydrofluoric acid have strong volatility and corrosive properties, protective equipment should be worn in accordance with the requirements of the regulations, and the process of solution preparation and sample pre-processing operated in the fume hood.   3.2 The 10% ammonium chloride solution needs to be added to the standard solution and the sample simultaneously to ensure the consistency of the testing.   4. Conclusion From the experimental results, the linear correlation coefficients of the lead, cadmium and chromium are all greater than 0.999. Lead and cadmium were not detected in the waste resin powder. Chromium was detected. The method is accurate, reliable, sensitive and can be used for the detection of heavy metals in waste resin powder.      
2024-09-20
Determination of Menthol Content in Mint by Gas Chromatogaphy
Determination of Menthol Content in Mint by Gas Chromatogaphy
  Determination of Menthol Content in Mint by Gas Chromatogaphy   In this paper, the chromatographic conditions are optimized with reference to the 2020 edition of the Chinese Pharmacopoeia, and a chromatographic column SK-WAX is used for the determination of menthol content in mint.   Keyword: Gas Chromatograph. FID Detector, Mint, Menthol   1. Experiment Method   1.1 Instrument Configuration Table 1 Configuration List of Gas Chromatography No Module Qty 1 GC6000 Gas Chromatography 1 2 FID6000 Detector 1 3 ASL6000 Autosampler 1   1.2 Test Conditions Chromatography Column: SK-WAX, 30m*0.32mm*0.25μm Temperature-Programmed: Keep the column at an initial temperature of 70°C for 4 minutes, heat up to 120°C at a rate of 1.5°C per minute, then to 200°C at a rate of 3°C per minute, and finally to 230°C at a rate of 30°C per minute and keep for 2 minutes; Carrier Gas: high purity nitrogen, constant Current Mode Column Flow Rate: 2mL/min Inlet Temperature: 200°C Detector Temperature: 300°C Hydrogen flow rate: 35mL/min Air Flow Rate: 300mL/min Injection Volume: 1μL Injection Method: Split-flow injection with a 5:1 split ratio.   1.3 Reagents and Experiment Material 1.3.1 Reagents Mint Sample Menthol Standard Ethanol, AR.   1.3.2 Equipment Needle Filter The third sieve   1.4 Sample Preparation 1.4.1 Preparation of Reference Solution Take the appropriate amount of menthol control, precision weighing, add ethanol to make a solution containing 0.2mg per 1mL.   1.4.2 Preparation of Test Solution Take 2g of product powder (through the third sieve), precision weighing, placed in a stoppered V-shaped bottle, and tightly stoppered after precision addition of 50mL of ethanol. Weighing, ultrasonic treatment (power 250W, frequency 33kHz) for 30 minutes, cooled, and then weighing. Make up the lost weight with ethanol, shake well, filter and take the subsequent filtrate.   2 Result and Communication 2.1 Chromatogram of Reference Solution Take the reference solution and analyzed according to the test conditions of 1.2, and the results are shown below. As shown in the figure and data, the peak shape is symmetrical, there is no other peaks, and the separation degree is higher than 1.5, which is good and met the requirements. Compound Retention Time Peak Area Peak Height Theoretical Plate Number Menthol 18.262 564.820 48.485 56284   Take the reference solution, injected and detected 7 times sequential according to the test conditions in 1.2, the repeatability chromatogram as shown below. According to the test results, the retentionr time repeatability of the reference solution is 0.021% and the peak area repeatability is 0.47%, and the test repeatability is good.     2.2 Chromatogram of Test Solution Take the test solution and analyzed according to the test conditions of 1.2, and the results as shown below. From the figure and the data, the peak shape is symmetrical, and there is no other peaks, and the separation degree is higher than 1.5, the separation is good and meets the requirements. Compound Retention Time Peak Area Peak Height Theoretical Plate Number Menthol 18.269 568.906 48.763 56738   Take the reference solution, injected and detected 7 times sequential according to the test conditions in 1.2, the repeatability chromatogram as shown below. According to the test results, the retention time repeatability of the reference solution is 0.038% and the peak area repeatability is 0.49%, and the test repeatability is good.   3. Conclusion In this paper, a method for the determination of menthol in mint is established by Wayeal gas chromatograph GC6000. The results showed that the menthol peaks in the chromatogram is symmetrical, the repeatability of the retention time of 7 injections is less than 0.5%, and the repeatability of the peak area is less than 0.5%, which showed a good test repeatability. The theoretical plate number is much higher than 10000, which meets the requirements of the Chinese Pharmacopoeia. This product is calculated according to the dry product, the content of menthol in the test sample is 0.50%, which meets the requirement of Pharmacopoeia of no less than 0.20%. This method can be a reference for the determination of menthol content in mint.                      
2024-09-19
Determination of Heavy Metals in soil by Atomic Absorption Spectrophotometer
Determination of Heavy Metals in soil by Atomic Absorption Spectrophotometer
  Determination of Heavy Metals in soil by Atomic Absorption Spectrophotometer   1. Experiment Method   Keywords: Atomic absorption spectrophotometer, autosampler, graphite furnace, flame, soil, heavy metals.   1.1 Instrument Configuration Table 1 Configuration Lists of AAS No Module Qty 1 Atomic Absorption Spectrophotometer AA2310 1 2 Graphite Furnace Power GF2310 1 3 Autosampler AS2310 1 4 Cooling Circulator 1 5 High Purity Argon 1 6 Graphite Tube 1 7 Oilless Air Compressor 1 8 High Purity Acetylene 1   1.2 Reagents and Experiment Material Nitric acid solution (1+99): Measure 10mL of nitric acid and slowly add to 990mL of water and mix well. Pb Standard Solution:1000mg/L Cd Standard Solution: 1000mg/L Ni Standard Solution: 1000mg/L 1% diammonium hydrogen phosphate: take 1g of diammonium hydrogen phosphate in a 100mL volumetric flask, and fix the volume with ultrapure water; Nitric Acid: GR Hydrochloric Acid: GR Hydrofluoric Acid: GR perchloric acid: GR One in ten thousand analytical balances Electrothermal blast thermostatic drying oven Digital display electric hot plate Teflon crucible   1.3 Sample Pretreatment Sample digestion: Weigh 0.2g of sample in a PTFE crucible, add one to two drops of water to moisten, add 10ml hydrochloric acid, 9ml nitric acid, 4ml hydrofluoric acid, and 2ml perchloric acid in turn, shake well, cover and heat on a hot plate at 150℃ for 6 hours, open the lid and continue to be heated in addition to silicon. In order to achieve a good effect of flying silica, it is necessary to shake the crucible frequently and drive the acid steaming until the content is viscous. Remove and cool slightly, add 0.5ml of nitric acid to dissolve the soluble residue, rinse the crucible lid and inner wall with water, transfer the whole amount to a 50ml volumetric flask, and fix the volume with ultrapure water, shake well. Store in PTFE reagent bottles for testing. Replace the sample with water and prepare a full program blank solution following the steps above. To be measured.   2. Conclusion and Discussion 2.1 Spectral Conditions for Lead   Heating Method Graphite Furnace Test Method Peak Height Injection Volume 20μL Sample + 5μL Diammonium Hydrogenphosphate Bandwidth 0.4nm Wavelength 283.3nm Ignite AA-BG Lamp Current 5mA   Concentration Table of Standard Curves (μg/L) Standard Curve 1 2 3 4 5 Leak Standard Solution 5.00 10.0 20.0 30.0 40.0 Standard Curve Testing   Linearity of Standard Curve    2.3 Spectral Conditions for Cadmium   Heating Method Graphite Furnace Testing Method Peak Height Injection Volume 15μL sample + 5μL 1% diammonium hydrogenphosphate Bandwidth 0.4nm Wavelength 228.8nm Ignite AA-BG Lamp Current 4mA   Concentration Table of Standard Curves (μg/L) Standard Curve 1 2 3 4 Cd Standard Solution 0.5 1.5 2.0 2.5 Standard Curve Testing   Linearity of Standard Curve   2.4 Spectral Conditions for Nickel   Heating Method Flame Burner Height 10mm Acetylene Flow Rate 2.0L/min Bandwidth 0.2nm Wavelength 232.0nm Ignite AA Lamp Current 4mA   Concentration Table of Standard Curve (μg/mL) Standard Curve 1 2 3 4 5 Ni Standard Curve 0.5 1.0 1.5 2.0 2.5 Standard Curve Testing   Linearity of Standard Curve   3. Calculation of Results   Sample No Sample Volume (g) Testing concentration Content(mg/kg) Theoretical Concentration (mg/kg) Standard Deviation Pb 1# 0.2005 16.2420μg/L 21 21±2 Qualified 1#- parallel 0.2009 17.6490μg/L Cd 1# 0.2005 0.4897μg/L 0.12 0.14±0.02 Qualified 1#- parallel 0.2009 0.4991μg/L Ni 1# 0.2005 0.1180μg/L 29 30±2 Qualified 1#- parallel 0.2009 0.1159μg/L   4. Note   Perchloric acid and nitric acid used in the experiment have strong oxidizing and corrosive properties, hydrochloric acid and hydrofluoric acid have strong volatility and corrosiveness, so reagent preparation and sample digestion should be carried out in a fume hood; protective equipment should be worn as required to avoid inhalation into the respiratory tract or contact with the skin and clothing during operation.  
2024-09-18
Determination of lbuprofen Extended-release Capsulesby High Performance Liquid Chromatography
Determination of lbuprofen Extended-release Capsulesby High Performance Liquid Chromatography
  Determination of lbuprofen Extended-release Capsulesby High Performance Liquid Chromatography   The analytical method presented herein, with reference to the determination of the content of ibuprofen extended-release capsules in the Pharmacopoeia of the People's Republic of China in the 2020 edition, was carried out on a Wayeal high-performance liquid chromatograph LC3200 series with a DAD detector.   1. Instrument Configuration and Experiment Method   1.1 Instrument Configuration   Table 1 Configuration List of Wayeal HPLC No Modular Qty 1 P3210Q Quaternary Pump 1 2 CT3210 Column Oven 1 3 AS3210 Autosampler 1 4 DAD3260 DAD 1 5 Nova Atom PC18 4.6*250mm, 5μm 1 6 SmartLab Workstation 1   1.2 Experiment Method   1.2.1 Preparation of Reagents No Reagents Purity 1 Methanol Chromatography Pure 2 Acetonitrile Chromatography Pure 3 Sodium Acetate AR 4 Glacial Acetic Acid GR   1.2.1.1 Test solution: take the contents under the loading difference, mix well, take appropriate amount (equivalent to about 0.1g of ibuprofen) into a 200mL measuring flask, add methanol 100mL, shaking for 30 minutes, dilute and fix the volume with water, sharking well, filtration, and remove the filtrate.   1.2.1.2 Reference Solution: Take 25mg of ibuprofen reference sample, weigh it precisely, put it in a 50mL measuring flask, add 25mL of methanol to make it dissolve, dilute and fix the volume with water, shake well.   1.2.1.3 Sodium acetate buffer solution: weigh 6.13g of sodium acetate, add 750mL of water to dissolve, and adjust the pH to 2.5 with glacial acetic acid.   1.2.2 Chromatography Conditions   Table 3 Chromatography Conditions Chromatography Colimn Nova Atom PC18, 4.6*250mm5μm Mobile Phase Ammonium acetate buffer solution Flow Rate 1mL/min Temperature 35°C Wavelength 263nm Injection Volume 20μL   2. Experiment Result   3.1 System Suitability Fig 1 Chromatogram of Sample Testing   Table 4 Test Data of Test Sample Sample Compound Retention Time Peak Area Peak Height Theoretical Pate Number Test Sample ibuprofen 4.778 1204.748 223.865 18650   Figure 2 Chromatogram of Reference Sample   Table 5 Test Data Reference Sample Sample Compound Retention Time Peak Area Peak Height Theoretical Pate Number Reference Sample ibuprofen 4.781 1515.707 280.794 18541   From the chromatogram and table, it can be seen that the peaks of the test sample and reference sample are good, there are no other peaks around the target peaks, and the theoretical plate numbers are all above 2500 in pharmacopoeia, which satisfied the experimental requirements.   3.2 Repeatability Fig 3 6 Injections Repeatability Chromatogram of Test Sample   Table 6 6 Injections Repeatability Data for Test Sample Sample No Retention Time Peak Area       Test Sample 1 4.778 1204.748 2 4.775 1205.853 3 4.778 1206.482 4 4.778 1206.091 5 4.781 1208.216 6 4.781 1209.01 RSD(%) 0.053 0.131     Fig 4 6 Injections Repeatability Chromatogram of Reference Sample   Table 7 6 Injections Repeatability Data for Reference Sample Sample No Retention Time Peak Area       Reference Sample 1 4.781 1515.707 2 4.781 1515.333 3 4.781 1518.024 4 4.781 1517.524 5 4.778 1515.806 6 4.778 1517.076 RSD (%) 0.036 0.073   Note: According to the data in the above table, the RSD of retention time for the test and reference sample are 0.053% and 0.036%, and the RSD of peak area is 0.131% and 0.073%, respectively. The repeatability results is good and satisfied the experimental requirements.   3.3 Sensitivity Testing Figure 5 Chromatogram of Test Sample Diluted 2000 Times   Table 8 Test Data for Test Sample Diluted 2000 Times Sample Compound Retention Time Peak Area Peak Area Signal-to-Noise Ratio Test Sample Diluted 2000 Times ibuprofen 4.795 0.597 0.133 4.600   Note: According to the data shown in the above table, the peak area of test sample diluted in 200 times is 0.597 with a signal-to-noise ratio of 4.6, which is a good test result and meets the experimental requirements.   4. Notes Glacial acetic acid has a strong irritating odor, so be careful to prepare the solution in a fume hood.   5. Conclusion The analytical method presented herein, with reference to the determination of the content of ibuprofen extended-release capsules in the Pharmacopoeia of the People's Republic of China in the 2020 edition, was carried out on a Wayeal high-performance liquid chromatograph LC3200 series with a DAD detector. The experimental results showed that the peak shape of the system adaptability test is good, and there are no other peaks around the target peak, and the theoretical plate number is above 2500, which meet the requirements of pharmacopoeia. The RSD of the retention time is 0.053% and 0.036% and the RSD of peak area is 0.131% and 0.073% for ibuprofen test sample and reference sample. Repeatability results are good. The sensitivity test result of 2000 times dilution of the test material is good. All the above results meet the requirements of the pharmacopoeia method.            
2024-09-14
Determination of Sulfur Dioxide in Chenpi Samples by Ion Chromatography
Determination of Sulfur Dioxide in Chenpi Samples by Ion Chromatography
Determination of Sulfur Dioxide in Chenpi Samples by Ion Chromatography   Ion chromatography has always been a research hotspot for the detection of sulfur dioxide in Chinese herbal, with its simple operation, high sensitivity and wide linear range, which is of practical value for the control of sulfur dioxide residue in pharmaceuticals.   In this experiment, the steam distillation method and the ion chromatography will be used to determine the content of sulfur dioxide in Chenpi. Wayeal ion chromatograph with conductivity detector, and KOH eluent. The method is simple to handle, with good recovery and high sensitivity, and is suitable for the determination of sulfur dioxide in Chenpi.   Keywords: Chenpi, sulfur dioxide, ion chromatograph   1. Experiment   1.1 Instruments and Reagents Ion Chromatography: IC6200 Series ion chromatography with conductivity detector Autosampler: AS2800 Anion Chromatography Column: HS-5A-P2, 250MM x 4.6mm, Sulfate ions in water(1000mg/L) 30% H2O2 solution; Concentrated Hydrochloric Acid: Guaranteed reagent Disposable Syringes (2mL) Water-based Syringe Filter (0.22μm) Electronic Balance, 1/10,000 The experimental water is prepared by the Wayeal ultrapure water purifier with a conductivity of 18.2 MΩ·cm (25 ℃).   1.2 Working Conditions Column Temperature: 35°C Cell Temperature : 40°C Eluent : 30Mm KOH isocratie elution Flow Rate : 1.0 mL/min Suppressor Current: 90mA Injection Volume: 25μL   1.3 Schematic Diagram of Steam Distillation 1.4 Sample Pretreatment Take appropriate amount of sample (accurate to 0.0001g) to bottle A (two-necked flask), add 50mL deionized water, shaking, so that the dispersion is uniform, then connected to the water vapor distillation flask C. 20mL of 3% hydrogen peroxide solution was absorbed in Bottle B. The lower end of the absorbing tube was inserted below the level of the absorbing solution. Add 5mL of hydrochloric acid along the wall of bottle A, quickly close the stopper, and begin distillation, keeping bottle C boiling and adjusting the distillation fire so that the effluent from the end of the absorber tube flows at a rate of about 2mL/min. Distill until the total volume of the solution in bottle B was about 95mL (30~40min), wash the tail pipe with water and transfer it to a volumetric flask, fix the volume to the scale, shake it well, let it stand for 1h, filtered through 0.22μm aqueous filter membrane, choose the appropriate dilution times, and test and analyze it on the machine.   2. Result and Discussion   2.1 Linearity Test 0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L, 2.0mg/L, 3.0mg/L of standard working curves of were pipetted respectively, and you will get the multi-point overlap chromatography of the standard curve according to the 1.2 working conditions, as shown in Fig. 1, linear equations as shown in Table1, and the linear correlation coefficients of sulfate under this chromatographic condition is above 0.999, which is good linearity.   Fig1 Overlap Chromatogram of SO4 Standard Curve   Fig 2 Standard Curve of SO4   Table 1 Linear Equation of Standard curve No Ions Linear Equation Correlation Coefficient R 1 So42- y=14.32737x-0.76329 0.99926   2.2 Sample Testing 2.2.1 Sample Content Testing The pre-treated samples were detected under the 1.2 working conditions. The sample chromatogram as shown in Fig. 3 and Fig. 4, the chromatographic peaks are symmetrical, with good separation and no other peaks, and the final content of sulfur dioxide in the sample as shown in Table 2.   Fig 3. Chromatogram of Sample 1   Fig 4. Chromatogram of Sample 2   Table 2 Sample Results Analysis Sample Weighing Sample/g Ions Concentration(mg/L) SO2 Content(g/kg) Blank / SO42- 0.272 / Sample 1 2.5551 SO42- 1.417 0.030 Sample 2 2.2370 SO42- 0.920 0.019     2.2.2 Sample Repeatability Testing Fig 4 Repeatability Chromatogram of Sample 1   Table 3 Repeatability Results of Sample 1 Sample Weighing Sample/g Retention Time/min Peak Area Concentration mg/L Sample 1 2.5551 12.307 19.615 1.422 12.290 19.627 1.423 12.267 19.327 1.402 12.250 19.632 1.424 12.230 19.380 1.406 12.247 19.640 1.424 Average Value 12.265 19.537 1.417 RSD% 0.235 0.732 0.705     3. Conclusion An ion chromatographic method was established for the determination of sulfur dioxide in Chenpi samples by using Wayeal IC6200 series ion chromatograph equipped with a conductivity detector. The samples were pre-treated and then separated by an ion chromatographic column and quantified by external standard method, which was able to qualitatively and quantitatively analyze the sulfur dioxide in Chenpi. The method is simple and easy to use, with good reproducibility, sensitivity and accuracy, which can be adopted for the determination of sulfur dioxide in Chenpi.
2024-09-13
Determination of Heavy Metals in Waste Resin Powder by Wayeal Atomic Absorption Spectrophotometer
Determination of Heavy Metals in Waste Resin Powder by Wayeal Atomic Absorption Spectrophotometer
  Determination of Heavy Metals in Waste Resin Powder by Wayeal Atomic Absorption Spectrophotometer   In this paper, with reference to the standard of "HJ 749-2015 Determination of Total Chromium in Solid Waste Flame Atomic Absorption Spectrophotometry" "HJ 786-2016 Determination of Lead, Zinc and Cadmium in Solid Waste Flame Atomic Absorption Spectrophotometry", an analytical method was established for the determination of the content of heavy metal elements in waste resin powder by flame atomic absorption method.   Keywords: Atomic Absorption Spectrophotometer; flame, waste resin powder; lead; cadmium; chromium.   1. Experiment Method   1.1 Instrument Configuration   Table 1 Configuration List of Atomic Absorption Spectrophotometer No Name Qty 1 Atomic Absorption Spectrophotometer AA2310 1 2 Air Compressor 1 3 High-purity Acetylene 1 4 Lead Hollow Cathode Lamp 1 5 Cadmium Hollow Cathode Lamp 1 6 Chromium Hollow Cathode Lamp 1   1.2 Reagents and Instruments 1.2.1 Lead Standard Solution(1000μg/ml) 1.2.2 Cadmium Standard Solution(1000μg/ml) 1.2.3 Chromium Standard Solution(1000μg/ml) 1.2.4 Ammonium Chloride: AR 1.2.5 Nitric Acid: GR 1.2.6 Hydrochloric Acid: GR 1.2.7 Hydrofluoric Acid: GR 1.2.8 Perchloric Acid: GR 1.2.9 30% Hydrogen Peroxide: GR 1.2.10 One in ten thousand analytical balances 1.2.11 Digital display electric hot plate   1.3 Pre-processing 1.3.1 Pre-processing of Lead and Cadmium Samples Take 0.2g of sample (accurate to 0.1mg) into a 50ml PTFE crucible. After wetting with water, 5ml of hydrochloric acid was added and the sample was heated on a hot plate in a fume hood at about 120 ℃ to initially disintegrate the sample, and then removed and cooled slightly after evaporation until about 3m remained. Add 8ml of nitric acid, 8ml of hydrofluoric acid and 4ml of perchloric acid, cover and heat at about 160 ℃ on a hot plate for 3h. Open the lid, the electric heating plate temperature control at 180 ℃ to continue heating, and often shake the crucible. When heated to a thick white smoke, cover to fully decompose the black organic carbons. After the black organic matter on the crucible wall disappears, open the lid, drive away the white smoke and steam until the contents are viscous. Take down the crucible, slightly cold, add 0.2mL nitric acid to dissolve the soluble residue, after cooling, transfer the whole amount to 50ml volumetric flask, rinse the crucible lid and inner wall with appropriate amount of experimental water, the washing solution was incorporated into 50ml volumetric flask, and the fix the volume with experimental water, shaken well, and then left to be measure. If there are undissolved particles in the digested solution, filtering and centrifugation or natural precipitation are required. (Note: Do not allow a lot of bubbles to come out when heating, otherwise it will cause loss of the sample.)   1.3.2 Pre-processing of Chromium Sample Take 0.2g (accurate to 0.0001g) of sample into a 50ml PTFE crucible. After wetting with water, 10ml of concentrated hydrochloric acid was added and the sample was heated on a hot plate in a fume hood at 50°C to initially decompose the sample. When evaporated to about 3ml, add 5ml of concentrated nitric acid, 5ml of hydrofluoric acid, cover and heat on the hot plate at about 120~130 ℃ for 0.5~1h, then open the lid, drive away the white smoke and steam until the contents are in the form of liquid beads in a non-flowing state (observe while hot). Depending on the condition of digestion, add 3ml of concentrated nitric acid, 3ml of hydrofluoric acid, 1ml of hydrogen peroxide, and repeat the above digestion process. Take down the crucible, slightly cold, add 0.2mL nitric acid to dissolve the soluble residue, transfer all the test solutions to a 50ml volumetric flask, add 5ml of 110% ammonium chloride solution, and fix the volume with experimental water, left to be measured. (Note: the total amount of 30% hydrogen peroxide added shall not exceed 10ml.)   2. Results and Discussion   Lead Detection Sample Lead Burner Hight 10mm Acetylene Flow Rate 2.0L/min Spectral Bandwidth 0.4nm Wavelength 283.3nm Lighting Way AA Lamp Current 5mA   Gradient Concentration Table (mg/L) of Lead Standard Curves and Sample Data Concentration Level 1 2 3 4 5 6 Concentration of Standard Solutions (mg/L) 0.5 1.0 2.0 4.0 8.0 10 Absorbance of Standard Solutions (abs) 0.0073 0.0136 0.0290 0.0578 0.1112 0.1353 Absorbance of Waste Resin Powder (abs) 0.0024 Concentration of Waste Resin Powder (mg/L) 0.0000 Lead Concentration of Waste Resin Powder (mg/kg) Not Detected   Standard Curve of Lead   Cadmium Detection Sample Cadmium Burner Height 10mm Acetylene Flow Rate 2.0L/min Spectral Bandwidth 0.4nm Wavelength 228.8nm Lighting Way AA Lamp Current 3mA   Gradient Concentration Table (mg/L) of Cadmium Standard Curve and Sample Data Concentration Level 1 2 3 4 5 Concentration of Standard Solutions (mg/L) 0.2 0.4 0.6 0.8 1.0 Absorbance of Standard Solutions (abs) 0.0667 0.0124 0.1775 0.2280 0.2748 Absorbance of Waste Resin Powder (abs) 0.0057 Concentration of Waste Resin Powder (mg/L) 0.0000 Cadmium Centration of Waste Resin Powder (mg/kg) Not Detected   Standard Curve of Cadmium Chromium Detection Sample Chromium Burner Height 10mm Acetylene Flow Rate 3.6L/min Spectral Bandwidth 0.2nm Wavelength 357.9nm Lighting Way AA Lamp Current 5mA   Gradient Concentration Table (mg/L) of Chromium Standard Curve and Sample Data Concentration Level 1 2 3 4 5 Concentration of Standard Solutions (mg/L) 0.2 0.4 0.6 0.8 1.0 Absorbance of Standard Solutions (abs) 0.0175 0.0388 0.0588 0.0786 0.0994 Absorbance of Waste Resin Powder (abs) 0.0130 Concentration of Waste Resin Powder (mg/L) 0.1519 Chromium Concentration of Waste Resin Powder (mg/kg) 37.7   Standard Curve of Chromium   3. Notes   3.1 Nitric acid and perchloric acid used in the experiment have strong oxidizing and corrosive properties, hydrochloric acid and hydrofluoric acid have strong volatility and corrosive properties, protective equipment should be worn in accordance with the requirements of the regulations, and the process of solution preparation and sample pre-processing operated in the fume hood.   3.2 The 10% ammonium chloride solution needs to be added to the standard solution and the sample simultaneously to ensure the consistency of the testing.   4. Conclusion   From the experimental results, the linear correlation coefficients of the lead, cadmium and chromium are all greater than 0.999. Lead and cadmium were not detected in the waste resin powder. Chromium was detected. The method is accurate, reliable, sensitive and can be used for the detection of heavy metals in waste resin powder.        
2024-09-12
Determination of Salidroside in Pharmaceuticals by High Performance Liquid Chromatography(HPLC)
Determination of Salidroside in Pharmaceuticals by High Performance Liquid Chromatography(HPLC)
Abstract   Purpose: Determination of Salidroside in Pharmaceuticals by High Performance Liquid Chromatography(HPLC) Method: C18 column, 4.6*250mm, 5μm; Wavelength: 275nm; Mobile Phase A: Water; mobile phase B: methanol; Flow Rate 1.0ml/min; Temperature: 30°C; Injection Volume: 5μl. A standard curve was established and the content of the target was calculated by the external standard method. Keywords: HPLC, UV Detector, Herbal, Salidroside   1. Experiment Method   1.1 Instrument Configuration     Wayeal LC3200 Series HPLC   No. Name Qty 1 LC3200 Series HPLC 1 2 P3200 Binary Pump 1 3 UV3200 Detector 1 4 CT3200 Column Oven 1 5 AS3200 Autosampler 1 Table 1 System Configuration of HPLC   1.2 Test Conditions Column: C18, 5μm, 4.6*250mm Temperature: 30°C Wavelength: 275nm Flow rate: 1.0ml/min Mobile phase: A: water; B: methanol Injection volume: 5μL   Gradient Condition: T (min) A Water (%) B Methanol (%) 0 95 5 15 90 10 35 85 15 36 95 5 50 95 5   1.3 Instrument, Reagents and Consumables Reagents: ultrapure water, Methanol(GR) Standards: Salidroside (99.7%) Auxiliary device: chemical balance; solvent filter; ultrasonic cleaners Experimental materials: filter membrane: aqueous phase filter membrane 0.45μm   1.4 Preparation of Solutions 1.4.1 Standard Solutions: Take appropriate amount of salidroside standard into a volumetric flask and dissolved in methanol to make the concentration of 0.0084125mg/mL, 0.016825mg/mL, 0.03365mg/mL, 0.0673mg/mL, 0.1346mg/mL, 0.2692mg/mL, 0.673mg/mL.   1.4.2 Sample Preparation: Take 1.0022g of sample 1 into a volumetric flask, add methanol and dissolve to 25mL. Take 1.0794g of sample 2 into a volumetric flask, add methanol and dissolve to 25mL.   2 Results and Discussion   2.1 System Suitability Fig 1 Chromatogram of Salidroside Standard   No Compound Retention Time Peak Area Peak Height Tailing Factor Theoretical Plate Number 1 Salidroside 36.262 812.469 31.885 1.035 45724 Table 2 Chromatography Parameters of Salidroside Standards   Analysis: The test results of salidroside were good with symmetrical peaks and high theoretical plate number.   2.2 Standard Curve Fig 2 Superimposed chromatogram of Salidroside Standard solutions   Fig 3 Curve Equation and Correlation Coefficient of Salidroside Standard Solutions   Analysis: The linear range of salidroside standard curve is good, r>0.999.   2.3 Repeatability Fig 4 Repeatability Chromatogram of Salidroside Standards (n=6)   No Sample Retention Time Peak Area 1 0.2692mg/L standard solution 36.265 807.365 2 36.262 812.469 3 36.247 812.562 4 36.224 815.145 5 36.228 813.374 6 36.272 814.529 Average   36.250 812.574 RSD(%)   0.055 0.340 Table 3 Repeatability Chromatographic Parameters Table of Salidroside (n=6)   Analysis: 6 injections of 0.2692 mg/L salidroside show good reproducibility, and the RSD value of retention time is 0.055% and the RSD value of peak area is 0.340%.   2.4 Sample 1   Fig 5 Chromatogram of Sample 1   No Compund Retention Time Peak Area Peak Height Tailing Factor Theoretical Plate Number concentration 1 Salidroside 36.201 185.337 7.335 1.038 47306 0.061933 mg/L Table 4 Chromatography Parameters of Sample 1   Analysis: The content of salidroside in the sample 1 was 0.061933 mg/L, which was calculated according to the standard curve equation.   2.5 Sample 2   Fig 6 Chromatogram of Sample 2   No Compound Retention Time Peak Area Peak Height Tailing Factor Theoretical Plate Number concentration 1 Salidroside 36.214 197.232 7.750 0.998 46217 0.065566 Table 4 Chromatography Parameters of Sample 2   Analysis: The content of salidroside in the sample 2 is 0.065566mg/L, which iscalculated according to the standard curve equation.   3. Conclusion   Wayeal LC3200 series high performance liquid chromatograph with UV detector is used to detect salidroside; the test result is good with symmetrical peaks and high theoretical plate number. The linear range of the standard curve is good, r>0.999. The repeatability is good and 6 injections of 0.2692 mg/L salidroside has good reproducibility, and the RSD value of retention time is 0.055% and the RSD value of peak area is 0.340%. The content of salidroside in sample 1 is 0.061933 mg/L, and the content of salidroside in sample 2 is 0.065566 mg/L, which are calculated according to the standard curve equation.            
2024-09-11
Guo Chengzhan, Secretary of Party Committee and Chairman of  China Environmental Protection Industry Association Visited Wayeal for Research and Guidance
Guo Chengzhan, Secretary of Party Committee and Chairman of China Environmental Protection Industry Association Visited Wayeal for Research and Guidance
Guo Chengzhan, Secretary of Party Committee and Chairman of China Environmental Protection Industry Association Visited Wayeal for Research and Guidance     On July 27th, Guo Chengzhan, Secretary of Party Committee and Chairman of China Environmental Protection Industry Association (CEPIA), and his delegation visited Wayeal for a research and discussion to understand the current situation of the enterprise and listen to the demands and suggestions.   In the seminar, Wayeal reported the development of the enterprise, the scientific research achievements and the future development plan. With the national "14th Five-Year Plan" and "Double Carbon" target, Wayeal actively responds to the needs of the country and enterprises, and launches "Digital Intelligence Double Carbon Integrated Solution", "Fine Particulate Matter - Ozone Synergy Control Solution", as well as comprehensive solutions in various scenarios such as air environment monitoring, water quality online monitoring, fixed pollution source monitoring and emergency monitoring.   During the exchange, President Guo Chengzhan affirmed the R&D strength and scientific research achievements of Wayeal, and highly praised its determination to attach importance to independent R&D and technological innovation in the past 20 years and insist on "not forgetting the original intention and replacing imports". He also said that with the high-quality development of ecological and environmental protection industry, the establishment of ecological and environmental monitoring and supervision system will slowly change from "human defense" to "technology defense". He hope that Wayeal will aim at the world's cutting-edge technology, play a leading role in the industry, adhere to scientific and technological innovation, and make greater contributions to the localization of high-end environmental monitoring instruments and equipment. After the meeting, Mr. Zang Mu, Chairman of Wayeal, took President Guo Chengzhan and his party to visit the exhibition hall, R&D lab and production workshop of Wayeal.
2022-08-03
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