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采用快速解析液相色谱-三重四极杆电喷雾串联质谱法同时测定元胡止痛片中 17 种成分的含量。

Simultaneous quantification of 17 constituents from Yuanhu Zhitong tablet using rapid resolution liquid chromatography coupled with a triple quadrupole electrospray tandem mass spectrometry.

机构信息

Institute of Chinese Materia Medica, China Academy of Chinese Medical Sciences, No. 16, Nanxiaojie, Dongzhimennei, Beijing 100700, PR China.

出版信息

J Pharm Biomed Anal. 2011 Nov 1;56(3):497-504. doi: 10.1016/j.jpba.2011.06.008. Epub 2011 Jun 16.

Abstract

A rapid resolution liquid chromatography coupled with a triple quadrupole mass spectrometry (RRLC-QQQ) was employed to identify and quantify the major bioactive constituents in Yuanhu Zhitong tablet (YZT), a traditional Chinese medicine. Seventeen constituents were simultaneously determined and quantified by reference standards in 9 min, namely scopoletin, protopine, α-allocryptopine, tetrahydropalmatine, coptisine, tetrahydroberberine, corydaline, berberine, byakangelicin, byakangelicol, xanthotoxin, bergapten, pimpinellin, oxypeucedanin, imperatorin, osthole and isoimperatorin. All of them were performed on an Agilent XDB C(18) column (4.6 mm × 50 mm, 1.8 μm) with linear gradient elution of acetonitrile-0.3% formic acid water (pH 2.7). The proposed method was applied to analyze 15 batches of samples with acceptable linearity (r(2), 0.9938-0.9999), precisions (RSD, 1.01-4.92%), repeatability (RSD, 1.33-4.91%), stability (RSD, 1.46-4.86%), recovery (RSD, 1.11-4.81%) of the seventeen compounds. Furthermore, the Hierarchical Cluster Analysis was applied to classify 15 samples based on characteristics of the 17 compound markers. As a result, the analytical method possessing high sensitivity and speed is suitable for the quality control of YZT.

摘要

采用快速解析液相色谱-三重四极杆串联质谱法(RRLC-QQQ)鉴定并定量分析元胡止痛片中的主要生物活性成分。通过参考标准,在 9 分钟内同时测定并定量了 17 种成分,即茴芹素、原阿片碱、α-allocryptopine、延胡索乙素、小檗碱、四氢巴马汀、紫堇灵、黄连碱、次野鸢尾黄素、次野鸢尾黄素甲醚、花椒毒素、补骨脂素、茴芹内酯、氧化吴茱萸碱、欧前胡素、蛇床子素和异欧前胡素。所有成分均在 Agilent XDB C(18)柱(4.6mm×50mm,1.8μm)上进行,采用乙腈-0.3%甲酸水(pH2.7)线性梯度洗脱。该方法应用于分析 15 批样品,具有可接受的线性(r(2),0.9938-0.9999)、精密度(RSD,1.01-4.92%)、重复性(RSD,1.33-4.91%)、稳定性(RSD,1.46-4.86%)和回收率(RSD,1.11-4.81%)。此外,应用层次聚类分析基于 17 种化合物标志物的特征对 15 个样品进行分类。结果表明,该分析方法具有高灵敏度和速度,适用于元胡止痛片的质量控制。

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