色谱

色谱 ›› 2016, Vol. 34 ›› Issue (8): 773-777.DOI: 10.3724/SP.J.1123.2016.03025

• 研究论文 • 上一篇    下一篇

高效液相色谱-质谱联用法同时测定脑心清原料药浸膏及其片剂中的8种有效成分

张梦雨1, 徐洋1, 宋冠杉2, 辛欣1, 彭缨1   

  1. 1. 沈阳药科大学, 辽宁 沈阳 110016;
    2. 沈阳市第二十七中学, 辽宁 沈阳 110016
  • 收稿日期:2016-03-17 出版日期:2016-08-08 发布日期:2016-07-26
  • 通讯作者: 彭缨

Simultaneous determination of eight effective constituents in Naoxinqing crude drug and tablets by high performance liquid chromatography-tandem mass spectrometry

ZHANG Mengyu1, XU Yang1, SONG Guanshan2, XIN Xin1, PENG Ying1   

  1. 1. Shenyang Pharmaceutical University, Shenyang 110016, China;
    2. Shenyang No. 27 High School, Shenyang 110016, China
  • Received:2016-03-17 Online:2016-08-08 Published:2016-07-26

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摘要：

建立了高效液相色谱-质谱联用（HPLC-MS/MS）同时测定脑心清原料药及其片剂中原儿茶酸、金丝桃苷、山柰酚-3-O-β-D-吡喃葡萄糖苷、山柰酚-3-O-β-D-吡喃半乳糖苷、杨梅素、槲皮素、柚皮素和山柰酚8种有效成分的分析方法。以乙腈和0.1%（v/v）甲酸水溶液为流动相进行梯度洗脱，经Dikma Diamonsil C18柱分离，采用电喷雾离子源以负离子多反应监测模式进行质谱检测。结果表明，8种有效成分在线性范围内线性关系良好（r > 0.99），回收率为99.0%~102.1%，相对标准偏差为0.9%~3.3%（n=6）。该方法高效、快速、准确，为脑心清原料药浸膏及其片剂的质量标准研究提供了一定的参考。

关键词: 高效液相色谱-质谱联用, 脑心清, 片剂, 有效成分, 原料药

Abstract:

A high performance liquid chromatography-tandem mass spectrometry method (HPLC-MS/MS) was developed for the determination of eight constituents in Naoxinqing crude drug and tablets, including protocatechuate, hyperoside, kaempferol-3-O-β-D-glucopyranoside, kaempferol-3-O-β-D-galactopyranoside, myricetin, quercetin, naringenin and kaempferol. Multiple reaction monitoring (MRM) with negative electrospray ionization (ESI-) in MS/MS was used for quantification. The eight compounds were separated on a Dikma Diamonsil C18 with the mobile phases of acetonitrile and 0.1% (v/v) formic acid aqueous solution with gradient elution. The eight compounds showed good linearity in their concentration ranges with the correlation coefficients (r) better than 0.99. The recoveries were from 99.0% to 102.1%, and the relative standard deviations (RSDs) were 0.9%-3.3% (n=6). The method is accurate, sensitive and effective. It can be used for the quality control of Naoxinqing crude drug and tablets.

Key words: crude drug, effective constituents, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), Naoxinqing, tablets

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