In addition to ibuprofen tablets, ibuprofen syrup also has the characteristics of fast absorption and benefit for children to take [1]. However, since ibuprofen is insoluble in water, and its syrup contains alkaline substances to increase its solubility [2, 3], it is no longer possible to determine the content of ibuprofen by the neutralization method specified in the Pharmacopoeia. In this paper, the content of ibuprofen syrup was determined by HPLC method, and satisfactory results were obtained.
1 Instruments and reagents Shimadzu LC-6A high-performance liquid chromatograph, SPD-6AV ultraviolet detector, SCL-6B system controller, C-R4A data processor, LC-6A infusion pump.
Ibuprofen reference substance: produced by Shandong Xinhua Pharmaceutical Factory, using this chromatographic condition to check for a single tailing peak. The former is rare. > Chromatographic peak, content is 99.80%; Ibuprofen syrup [3]: self-made, the marked amount is 2% (g.mL-1); diphenylamine (internal standard) and anhydrous methanol are analytically pure.
2 Chromatographic conditions Chromatographic column: YWG? C18 4.6 mm × 250 mm; mobile phase: take 380 mg of sodium dihydrogen phosphate and 50 mg of disodium hydrogen phosphate, add water to dissolve to 1000 mL, adjust pH to 3.0 with phosphoric acid, take out 250 mL and add 750 mL of methanol, mix well. Flow rate: 1 mL.min-1; detection wavelength 220 nm; injection volume 20 μL; detection sensitivity: 0.01 AUFS.
3 Preparation of standard curve Precisely weigh the appropriate amount of diphenylamine, add anhydrous methanol to make a solution of 0.7 mg.mL-1, and use it as an internal standard solution. Another appropriate amount of ibuprofen reference substance, accurately weighed, and add anhydrous methanol to make a solution of 0.27 mg.mL-1, as a reference solution. Precisely measure 0.5, 1.0, 1.5, 2.0, 2.5, 5.0 mL of the reference solution, place them in 50 mL measuring flasks respectively, add 1.0 mL of internal standard solution, dilute to the mark with anhydrous methanol, shake well, and inject 20 μL . The area composed of the baseline of the reference substance and the internal standard is called the peak area. A = × σ × h = 2.507σh = 1.064 Wh / 2h> The ratio of peak areas is the ordinate, and the corresponding reference substance concentration (mg.mL-1) is the abscissa. The regression equation is obtained: Y = 75.5X + 0.0136 r = The results of 0.9997 showed that the concentration of ibuprofen solution in the range of 3-30 μg.mL-1 had a good linear relationship with the peak area. Chromatograms of diphenylamine and ibuprofen Figure 1 Chromatograms of diphenylamine and ibuprofen 1. Diphenylamine 2. Ibuprofen 4 Recovery experiment Take the ibuprofen reference substance about 100 mg, weigh accurately, transfer quantitatively to 100 In a mL measuring flask, add simple syrup, L-arginine, sodium benzoate, and fragrance according to the prescription, dilute to the mark with anhydrous methanol, and shake well. Accurately take 1 mL each of the above solution and the internal standard solution, and operate according to the "Sample Determination" item. The measured average recovery rate was 99.89%, RSD was 0.93%, n = 6.
5 Determination of samples Take about 2.5 mL of ibuprofen syrup, weigh accurately, transfer quantitatively to a 50 mL measuring flask, dilute to the mark with anhydrous methanol, and shake well. Accurately draw 1 mL each of the above solution and the internal standard solution into a 50 mL volumetric flask, dilute to the mark with anhydrous methanol, shake well, and inject 20 μL. The measured sample content is 97.23% of the marked amount, n = 5, and RSD is 0.89%.
6 Discussion After the stability test observation, the sample solution was placed at room temperature (approximately 18 ℃) and measured every 2 hours to 6 hours. The RSD of the percentage content of the sample was 0.99%, n = 3. The sample solution is relatively stable.
With diazepam as the internal standard, the effect is also good. However, because the author wants to use this method for the bioavailability measurement of ibuprofen syrup, in order to prevent the interference of stable drugs in the human body, diphenylamine is selected as the internal standard.
This article is derived from the determination of the content of ibuprofen syrup by HPLC method | Scientific Instrument Online Text Link: http: //
1 Instruments and reagents Shimadzu LC-6A high-performance liquid chromatograph, SPD-6AV ultraviolet detector, SCL-6B system controller, C-R4A data processor, LC-6A infusion pump.
Ibuprofen reference substance: produced by Shandong Xinhua Pharmaceutical Factory, using this chromatographic condition to check for a single tailing peak. The former is rare. > Chromatographic peak, content is 99.80%; Ibuprofen syrup [3]: self-made, the marked amount is 2% (g.mL-1); diphenylamine (internal standard) and anhydrous methanol are analytically pure.
2 Chromatographic conditions Chromatographic column: YWG? C18 4.6 mm × 250 mm; mobile phase: take 380 mg of sodium dihydrogen phosphate and 50 mg of disodium hydrogen phosphate, add water to dissolve to 1000 mL, adjust pH to 3.0 with phosphoric acid, take out 250 mL and add 750 mL of methanol, mix well. Flow rate: 1 mL.min-1; detection wavelength 220 nm; injection volume 20 μL; detection sensitivity: 0.01 AUFS.
3 Preparation of standard curve Precisely weigh the appropriate amount of diphenylamine, add anhydrous methanol to make a solution of 0.7 mg.mL-1, and use it as an internal standard solution. Another appropriate amount of ibuprofen reference substance, accurately weighed, and add anhydrous methanol to make a solution of 0.27 mg.mL-1, as a reference solution. Precisely measure 0.5, 1.0, 1.5, 2.0, 2.5, 5.0 mL of the reference solution, place them in 50 mL measuring flasks respectively, add 1.0 mL of internal standard solution, dilute to the mark with anhydrous methanol, shake well, and inject 20 μL . The area composed of the baseline of the reference substance and the internal standard is called the peak area. A = × σ × h = 2.507σh = 1.064 Wh / 2h> The ratio of peak areas is the ordinate, and the corresponding reference substance concentration (mg.mL-1) is the abscissa. The regression equation is obtained: Y = 75.5X + 0.0136 r = The results of 0.9997 showed that the concentration of ibuprofen solution in the range of 3-30 μg.mL-1 had a good linear relationship with the peak area. Chromatograms of diphenylamine and ibuprofen Figure 1 Chromatograms of diphenylamine and ibuprofen 1. Diphenylamine 2. Ibuprofen 4 Recovery experiment Take the ibuprofen reference substance about 100 mg, weigh accurately, transfer quantitatively to 100 In a mL measuring flask, add simple syrup, L-arginine, sodium benzoate, and fragrance according to the prescription, dilute to the mark with anhydrous methanol, and shake well. Accurately take 1 mL each of the above solution and the internal standard solution, and operate according to the "Sample Determination" item. The measured average recovery rate was 99.89%, RSD was 0.93%, n = 6.
5 Determination of samples Take about 2.5 mL of ibuprofen syrup, weigh accurately, transfer quantitatively to a 50 mL measuring flask, dilute to the mark with anhydrous methanol, and shake well. Accurately draw 1 mL each of the above solution and the internal standard solution into a 50 mL volumetric flask, dilute to the mark with anhydrous methanol, shake well, and inject 20 μL. The measured sample content is 97.23% of the marked amount, n = 5, and RSD is 0.89%.
6 Discussion After the stability test observation, the sample solution was placed at room temperature (approximately 18 ℃) and measured every 2 hours to 6 hours. The RSD of the percentage content of the sample was 0.99%, n = 3. The sample solution is relatively stable.
With diazepam as the internal standard, the effect is also good. However, because the author wants to use this method for the bioavailability measurement of ibuprofen syrup, in order to prevent the interference of stable drugs in the human body, diphenylamine is selected as the internal standard.
This article is derived from the determination of the content of ibuprofen syrup by HPLC method | Scientific Instrument Online Text Link: http: //
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