高效液相色谱法同时测定人工牛黄甲硝唑胶囊中甲硝唑和胆红素含量  

Simultaneous Determination of Metronidazole and Bilirubin in Galculus Bovis and Metronidazole Capsules by HPLC

作　　者：陈路 李苗 黄金秋 兰彤 宫立孟 CHEN Lu;LI Miao;HUANG Jinqiu;LAN Tong;GONG Limeng(Wuhan Institute for Drug and Medical Device Control·NMPA Key Laboratory for Quality Research and Control of Pharmaceutical Preparation,Wuhan,Hubei,China 430075;Hubei Biological Medicine Industrial Technology Institute Co.,Ltd.,Wuhan,Hubei,China 430073)

机构地区：[1]武汉药品医疗器械检验所·国家药品监督管理局药物制剂质量研究与控制重点实验室,湖北武汉430075 [2]湖北生物医药产业技术研究院有限公司,湖北武汉430073

出　　处：《中国药业》2023年第22期95-98,共4页China Pharmaceuticals

基　　金：湖北省药品监督管理局科研项目[20200113]。

摘　　要：目的 建立同时测定人工牛黄甲硝唑胶囊中甲硝唑和胆红素含量的高效液相色谱法。方法 色谱柱为Hypersil BDS C18柱(200 mm×4.6 mm,5μm),流动相为1%醋酸水溶液-乙腈(梯度洗脱),流速为1 mL/min,检测波长分别为449 nm(胆红素)和320 nm(甲硝唑),柱温为30℃,进样量分别为10μL(甲硝唑)和5μL(胆红素)。结果 胆红素、甲硝唑质量浓度分别在1.98~13.85μg/mL和20.13~201.28μg/mL范围内与峰面积线性关系良好(r=0.999 9,n=7);定量限分别为0.10μg/mL和0.057μg/mL;精密度、稳定性、重复性试验结果的RSD均不超过1.0%;平均加样回收率分别为99.50%和99.76%,RSD分别为0.82%和0.48%(n=9)。结论 该方法专属性强、精密度好、准确性高、操作简便,可用于同时测定人工牛黄甲硝唑胶囊中甲硝唑和胆红素的含量。Objective To establish a high-performance liquid chromatography(HPLC)method for the simultaneous determination of metronidazole and bilirubin in Galculus Bovis and Metronidazole Capsules.Methods The chromatographic column was Hypersil BDS C18 column(200 mm×4.6 mm,5μm),the mobile phase was 1%acetic acid aqueous solution-acetonitrile(gradient elution),the flow rate was 1 mL/min,the detection wavelength was 449 nm(bilirubin)and 320 nm(metronidazole)respectively,the column temperature was 30℃,and the injection volume was 10μL(metronidazole)and 5μL(bilirubin)respectively.Results The linear ranges of bilirubin and metronidazole were 1.98-13.85μg/mL and 20.13-201.28μg/mL(r=0.9999,n=7)respectively.The limits of quantitation of the above two components were 0.10μg/mL and 0.057μg/mL respectively.The RSDs of precision,stability and repeatability tests were not higher than 1.0%.The average recovery rates of bilirubin and metronidazole were 99.50%and 99.76%,with RSDs of 0.82%and 0.48%respectively(n=9).Conclusion This method is specific,precise,accurate and simple,which can be used for the simultaneous determination of metronidazole and bilirubin in Galculus Bovis and Metronidazole Capsules.

关 键 词：人工牛黄甲硝唑胶囊 甲硝唑 胆红素 高效液相色谱法 含量测定 

分 类 号：R917[医药卫生—药物分析学] R927[医药卫生—药学]