HPLC法同时测定银黄制剂中9个成分的含量  

Simultaneous determination of nine components in Yinhuang preparations by HPLC

作　　者：韩强[1] 陈辉 李银洁[3] 杨冬芝[3] 江相兰[3] 汤道权[3] 

机构地区：[1]徐州医学院附属医院药剂科,徐州221002 [2]徐州市食品药品检验所,徐州221002 [3]徐州医学院药物分析教研室,徐州221004

出　　处：《药物分析杂志》2013年第10期1686-1692,共7页Chinese Journal of Pharmaceutical Analysis

基　　金：江苏省奥赛康临床药学基金(201012);徐州市科技计划项目(XX10A52)

摘　　要：目的:建立同时测定银黄制剂中9个成分(绿原酸、咖啡酸、木犀草苷、黄芩苷、木犀草素、汉黄芩苷、黄芩素、汉黄芩素、千层纸素A)含量的高效液相色谱方法。方法:采用Sepax GP-C18色谱柱(250 mm×4.6 mm,5μm),以0.1%甲酸甲醇溶液-0.1%甲酸水溶液为流动相,梯度洗脱,流速1.0 mL·min-1,黄芩苷、汉黄芩苷、黄芩素、汉黄芩素、千层纸素A的检测波长为275 nm,绿原酸和咖啡酸的检测波长为320 nm,木犀草苷和木犀草素的检测波长为350 nm,柱温30℃,进样量20μL;液质联用法确认化合物的结构。结果:9个成分在考察的浓度范围内,浓度与峰面积之间呈良好的线性关系(r>0.9997);回收率(n=9)均在97.1%～103.9%范围内,RSD均小于2.6%。批内精密度RSD均小于1.0%,批间精密度RSD均小于1.7%。结论:本方法简便、准确,精密度高,重复性好,可用于银黄制剂的质量控制。Objective： To establish an HPLC method for simultaneous determination of nine components（chlorogenic acid,caffeic acid,luteoloside,baicalin,luteolin,wogonoside,baicalein,wogonin and oroxylin A）in Yinhuang preparations. Methods： The chromatographic separations were obtained on a Sepax GP-C18 column（250 mm×4.6 mm,5 μm）with a gradient elution using the mixture of 0.1% formic acid methanol solution and 0.1% formic acid water solution at a flow rate of 1.0 mL·min-1.The detection wavelengths were respectively set at 275 nm（baicalin,wogonoside,baicalein,wogonin and oroxylin A）,320 nm（chlorogenic acid and caffeic acid）and 350 nm（luteoloside and luteolin）.The column temperature was set at 30℃.The injection volume was 20 μL.The constituents were confirmed by（-）electrospray ionization LC-MS. Results： All calibration curves were linear（r 〉0.9997）over the tested ranges.The average recoveries（n=9）ranged from 97.1% to 103.9% with RSD value below 3.0%.The RSDs of within-run and between-run precision were below 1.0% and 1.7%,respectively. Conclusion： The established method is simple,fast,and with high precision,sensitivity and repeatability,which can be used efficiently in the quality control of Yinhuang preparations.

关 键 词：高效液相色谱法 液质联用法 银黄制剂 含量测定 绿原酸 咖啡酸 木犀草苷 黄芩苷 木犀草素 汉黄芩苷 黄芩素 汉黄芩素 千层纸素A 中成药质量控制 

分 类 号：R917[医药卫生—药物分析学]