2024-09-14
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 | ||
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.
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