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采用超高效液相色谱-三重四极杆质谱联用技术快速同时测定片仔癀中 12 种主要成分。

Rapid simultaneous determination of twelve major components in Pien Tze Huang by ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry.

出版信息

J Sep Sci. 2013 Dec;36(24):3866-73. doi: 10.1002/jssc.201300655.

Abstract

An efficient method using ultra-performance LC coupled with triple quadrupole MS was developed for the rapid determination of 12 major active components in Pien Tze Huang (PZH), a well-known traditional Chinese formula. Chromatographic separation was achieved on a Waters XBridge BEH RP18 column (50 mm × 2.1 mm id, 1.7 μm) with a gradient mobile phase (A: 0.1% aqueous formic acid and B: acetonitrile with 0.1% formic acid) at a flow rate of 0.8 mL/min. The chromatographic peaks of 12 components were identified by comparing their retention time and MS data with the related reference compounds. Multiple-reaction monitoring was employed for the quantitative analysis. Ten batches of PZH were analyzed with a good linear regression relationship (r, 0.9987–0.9995), intraday precisions (RSD, 2.05–4.80%), interday precisions (RSD, 1.99–4.98%), repeatability (RSD, 2.21–4.20%), stability (RSD, 3.52–4.81%), and recovery (95.63–104.80%). By using this established method, the present study offered highly sensitive, specific, and speedy determination of 12 major components, which promoted the quality control investigation of PZH greatly.

摘要

建立了一种超高效液相色谱-三重四极杆串联质谱联用的快速测定方法,用于测定著名的中药配方片仔癀中的 12 种主要活性成分。采用 Waters XBridge BEH RP18 柱(50mm×2.1mmid,1.7μm),以 0.1%甲酸水溶液(A)和含 0.1%甲酸的乙腈(B)为流动相进行梯度洗脱,流速为 0.8mL/min。通过比较保留时间和质谱数据与相关对照品,鉴定了 12 个成分的色谱峰。采用多反应监测模式进行定量分析。对 10 批片仔癀进行分析,具有良好的线性回归关系(r,0.9987-0.9995)、日内精密度(RSD,2.05%-4.80%)、日间精密度(RSD,1.99%-4.98%)、重复性(RSD,2.21%-4.20%)、稳定性(RSD,3.52%-4.81%)和回收率(95.63%-104.80%)。采用该方法可灵敏、特异、快速地测定 12 种主要成分,为片仔癀的质量控制研究提供了有力支持。

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