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复方蒿甲醚分散片的溶出度研究及其方法学验证

鲁素雅,邢海艳,金鹏,袁耀佐,金华   

  1. 淮安市食品药品检验所,淮安市食品药品检验所,淮安市食品药品检验所,江苏省食品药品监督检验研究院,淮安市食品药品检验所
  • 收稿日期:2018-11-20 修回日期:2019-01-29 出版日期:2019-02-25 发布日期:2019-02-25

A Method for Determining the Dissolution of Artemether and Lumefantrine

  1. Huai''an Institute for Food and Drug Control,,,,
  • Received:2018-11-20 Revised:2019-01-29 Online:2019-02-25 Published:2019-02-25

摘要: 建立并验证复方蒿甲醚分散片中蒿甲醚和苯芴醇的溶出度测定方法。方法:蒿甲醚的溶出以水1 000 mL为溶出介质,桨法,转速为100 r·min-1,于 1 h和3 h取样测定,用十八烷基硅烷键合硅胶为填充剂(Macherey-Nagel,Nucleosil 100-5,12.5 cm ×40 mm),以水-乙腈-正丙醇-三氟乙酸(400∶500∶100∶1)为流动相,检测波长为 210 nm,流速为1mL·min-1;蒿甲醚检测波长为 210 nm。苯芴醇的溶出以 1%氯化苄基二甲基烷基胺的0.1 mol·L-1盐酸溶液 1 000 mL为介质,桨法,转速为100 r·min-1,45 min时取样测定,按吸收系数法(E1%1 cm)在 342 nm 波长处测定吸光度。结果:蒿甲醚在1 h和3 h的溶出分别为58.5%和85.9%以上;苯芴醇在45 min溶出82.8%以上。结论:该方法分别测定分散片中蒿甲醚和苯芴醇的溶出度,稳定性高,专属性强。

Abstract: To establish and validate the method for determining the dissolution of artemether and lumefantrinein the artemether and lumefantrinedispersible tablets.Methods: For artemether, using 1 000 mL of degassed water as the dissolution medium, and rotating the paddle at 100 revolutions per minute. At 60 minutes and 180 minutes withdraw a sample of 10 mL of the medium through an in-line filter as test solutions. Using a stainless steel column (12.5 cm×40 mm) packed withparticles of silica gel which has been modified with chemically bonded octadeylsilyl groups (Macherey-Nagel,Nucleosil 100-5 was recommended). As the mobile phase, use a mixture of 400 volumes of water, 500 volumes of acetonitrile 100 volumes of 1-propanol and 1 volume of trifluoroacetic acid.Operate with a flow rate of 1 mL per minute. As a detector using an ultraviolet spectrophotometer was set at a wavelength of about 210 nm.For lumefantrine, using 1000 ml of hydrochloric acid (~3.6 g·L-1) TS, 1% benzalkonium chloride Ras the dissolution medium, and rotating the paddle at 100 revolutions per minute. At 45 minutes withdraw a sample of 10 ml of the medium through an in-line filter.Allow the filtered sample to cool to room temperature. Measure the absorbance of a 1 cm layer of the resulting solution, suitably diluted if necessary, at the maximum at about 342 nm. For each of the six tablets tested, calculate the total amount of lumefantrine (C30H32Cl3NO) in the medium, using the absorptivity value of 300.8(A1%1 cm=300.8). Results:The dissolution of artemether at 1 hour and 3 hours wasabove58.5% and 85.9%, respectively; Lumefantrinewas dissolved above 82.8% at 45 minutes. Conclusion:The methods to determine the dissolution of artemether and lumefantrinein the artemether and lumefantrine dispersible tablets, and which is accurate, high in stability and strong in specificity.