基于多成分定量分析结合薄层色谱检查的颠茄流浸膏质量评价  

Quality Evaluation of Belladonna Liquid Extract by Multicomponent Quantitation and TLC

作　　者：王迅[1] 黄巧玲[1] 张文婷 WANG Xun;HUANG Qiaoling;ZHANG Wenting(Hangzhou Third Hospital,Hangzhou 310009,China;Zhejiang Institute for Food and Drug Control,Hangzhou 310052,China)

机构地区：[1]杭州市第三人民医院,杭州310009 [2]浙江省食品药品检验研究院,杭州310052

出　　处：《中国现代应用药学》2020年第2期187-191,共5页Chinese Journal of Modern Applied Pharmacy

摘　　要：目的建立颠茄流浸膏中同时测定4种指标成分含量的方法,结合薄层色谱检查,为其质量评价提供依据。方法采用HPLC,色谱柱:Agilent Kromesil 100-5 C18柱(4.6 mm×250 mm,5μm),流动相为甲醇-0.05%甲酸溶液,梯度洗脱,流速1.0 mL·min^-1,柱温为30℃。采用薄层色谱法进行阿托品检查。结果 4种活性成分东莨菪苷在0.065 76~0.657 6μg(r=1.000 0)、山柰酚-3-O-半乳糖-(6→1)鼠李糖-7-O-葡萄糖苷在0.082 16~0.821 6μg(r=0.999 9)、东莨菪内酯在0.049 84~0.498 4μg(r=1.000 0)和芦丁在0.010 00~0.099 98μg(r=0.999 9)内,均呈良好线性关系;东莨菪苷、山柰酚-3-O-半乳糖-(6→1)鼠李糖-7-O-葡萄糖苷、东莨菪内酯和芦丁的加样回收率分别为100.6%,99.8%,99.9%和97.9%,RSD分别为1.4%,1.6%,1.4%和1.5%。部分批次指标成分含量低且检出硫酸阿托品。结论建立的含量测定方法灵敏度高,结果准确,适用于颠茄流浸膏的质量评价。OBJECTIVE To establish a method of the simultaneous determination of 4 components in Belladonna liquid extract,provide the basis for its quality evaluation by combing with TLC.METHODS Adopting HPLC and using Agilent Kromesil 100-5 C18 chromatographic column(4.6 mm × 250 mm,5 μm),the mobile phase was a mixture of acetonitrile and 0.05% formic acid for gradient elution.The flow rate was 1.0 mL·min^-1.The temperature of column was 30 ℃.Atropine sulfate was identified with TLC method.RESULTS Four active ingredients had good linear relationships:scopolin was in the range of 0.065 76-0.657 6 μg(r=1.000 0),kaempferol-3-O-galactosyl(6→1)-rhamnosyl-7-O-glucoside was in the range of 0.082 16-0.821 6 μg(r=0.999 9),scopoletin was in the range of 0.049 84-0.498 4 μg(r=1.000 0) and rutin was in the range of 0.010 00-0.099 98 μg(r=0.999 9).The average recoveries of scopolin,kaempferol-3-O-galactosyl(6→1)-rhamnosyl-7-O-glucoside,scopoletin and rutin were 100.6%,99.8%,99.9% and 97.9%.And their RSDs were 1.4%,1.6%,1.4% and 1.5%.The contents of some ingredients were low and atropine sulfate was detected in some samples.CONCLUSION This method has high sensitivity,it is accurate and suitable for the quality control of Belladonna liquid extract.

关 键 词：颠茄流浸膏 东莨菪苷 山柰酚-3-O-半乳糖-(6→1)鼠李糖-7-O-葡萄糖苷 东莨菪内酯 芦丁 硫酸阿托品 

分 类 号：R917.101[医药卫生—药物分析学]