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Objective: To optimize the formulation of the self-emulsifying drug delivery system of total saponins of Sanguisorba officinalis and evaluate its characteristics. Methods: The formulation and its proportion of the self-emulsifying drug delivery system of total saponins of S. officinalis were optimized based on the solubility tests, formula compatibility, microemulsion area in the ternary phase diagram and D-optimal mixing experiment design. The dosage of oil phase, surfactant and co-surfactant were investigated by drug loading, particle size, and polydispersity index. The appearance, particle size, polydispersity index, Zeta potential, and in vitro release of preparation were finally evaluated. Results: The ratio of oil phase, surfactant, and co-surfactant was 0.25: 0.45:0.30. The drug loading was 23.93 mg/g, the average particle size was (207.92 ± 2.13) nm and the zeta potential was (38.84 ± 0.18) mV. The release of SEDDS was superior to the bulk drug apparently. Conclusion: The self-emulsifying drug delivery system of total saponins of S. officinalis was established. The technology was feasible and the quality was stable.
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Objective To establish a method to determine genotoxic impurities in saxagliptin bulk drug. Methods The gas chromatography(GC) was carried out with INNOWAX capillary column. The inlet temperature was 120°C. The injection volume was 5 µl and separation ratio was 1:10. The column temperature was programmed: the initial temperature was 70°C, maintained for 1 min, raised to 190°C with a rate of 16 °C/min, and then maintained for another 5 min. The detector was flame ionization detector(FID), with temperature of 250°C. The carrying gas was N2 with the flow rate of 1 ml/min. Methanol was used as solvent for saxagliptin. Results Methyl mesylate, ethyl mesylate and isopropyl mesylate could be separated completely with good linear relationship between 2.44- 36.6, 2.38-35.7 and 2.46-36.9 µg/ml, respectively. The average recovery was 96.94%, 95.96% and 105.47%(n=9), respectively. Conclusion This method is simple, reproducible and accurate enough for the determination of genotoxic impurities in saxagliptin bulk drug.
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Objective To establish a method to determine genotoxic impurities in saxagliptin bulk drug. Methods The gas chromatography(GC)was carried out with INNOWAX capillary column. The inlet temperature was 120℃. The injection volume was 5μl and separation ratio was 1∶10. The column temperature was programmed:the initial temperature was 70℃,maintained for 1 min, raised to 190℃with a rate of 16℃/min,and then maintained for another 5 min. The detector was flame ionization detector(FID),with temperature of 250℃. The carrying gas was N2 with the flow rate of 1 ml/min. Methanol was used as solvent for saxagliptin. Results Methyl mesylate,ethyl mesylate and isopropyl mesylate could be separated completely with good linear relationship between 2.44-36.6,2.38-35.7 and 2.46-36.9μg/ml,respectively. The average recovery was 96.94%,95.96%and 105.47%(n=9),respectively. Conclusion This method is simple,reproducible and accurate enough for the determination of genotoxic impurities in saxagliptin bulk drug.
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OBJECTIVE: To determine and compare the contents of principal component and related substances of ammonium glycyrrhizinate by methods contained in different pharmacopoeias and a new method established by our lab. METHODS: The methods for quality control of ammonium glycyrrhizinate in the latest edition of European Pharmacopoeia, British Pharmacopoeia, national drug standards of China, and the method established by our laboratory were employed to determine the contents of the principal component isomers and related substances of ammonium glycyrrhizinate in its raw materials and pharmaceutical products. The methods were evaluated and compared regarding the chromatographic features, resolution of principal component isomers, experimental cost, content determination results, and the advantages and disadvantages of each method were discussed. RESULTS: The mobile phases adopted in aforementioned pharmacopoeias are all acidic, which could not effectively separate 18α-glycyrrhizinic acid and 18β-glycyrrhizinic acid, thus could not truly reflect the contents of 18α-glycyrrhizinic acid, 18β-glycyrrhizinic acid, related substances A, and the related substances in the raw materials and pharmaceutical products. The resolution of principal component isomer by our method was 1.5, complying to the pharmacopoeia requirement. The content determination results of ammonium glycyrrhizinate raw materials by the four methods had no significant difference. CONCLUSION: Among the four methods, the method established by our laboratory performed best in terms of accuracy and practicability. This method has shorter detection time, lower cost, reduced toxicity and pollution, and the results are accurate and reliable, which suggests that it can be used for the chiral resolution of 18α-glycyrrhizinic acid and 18β-glycyrrhizinic acid and the content determination of principal component and related substances of the raw material and pharmaceutical products of ammonium glycyrrhizinate. This study provideds reference for further revision of the quality control method in Pharmacopoeia.
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OBJECTIVE: To establish an HPLC gradient elution method for the determination of related substances in fluconazole bulk drug. METHODS: The separation was achieved by using an ODS column with gradient elution of mobile phase composed of 0.01 mol · L-1 ammonium formate and acetonitrile. The flow rate was 0.5 mL · min-1. The UV detection wavelength was 261 nm, injection volume is 20 μL. RESULTS: Fluconazole and its related substances can be separated effectively by this method, linear relation of fluconazole and impurity B-D were good, the detection limit were 0.20, 0.0052, 0.0073, 0.13 μg · mL-1, seventeen batches sample from nine manufacturers were determined. The related substances in fluconazole bulk drug were effectively determined. CONCLUSION: The HPLC method is rapid and accurate which may be used for the inspection of related substances in fluconazole bulk drug. Copyright 2012 by the Chinese Pharmaceutical Association.