色谱 ›› 2018, Vol. 36 ›› Issue (4): 408-412.DOI: 10.3724/SP.J.1123.2017.11002

• 技术与应用 • 上一篇    下一篇

超高效液相色谱-串联质谱法测定阿胶中马、牛、羊、猪、骆驼、鹿皮源成分

杭宝建1, 田晨颖2, 陈晓1, 邢晟1, 石峰1, 冷佳蔚1, 巩丽萍1   

  1. 1. 山东省食品药品检验研究院, 山东 济南 250101;
    2. 山东中医药大学, 山东 济南 250355
  • 收稿日期:2017-11-03 出版日期:2018-04-08 发布日期:2014-02-26
  • 通讯作者: 石峰,Tel:(0531)81216561,E-mail:13953175123@163.com;冷佳蔚,E-mail:sdsypjys@163.com;巩丽萍,E-mail:gongliping_lp@163.com
  • 基金资助:

    国家重大新药创制专项(2014ZX0930437).

Determination of the ingredients of horse, ox, sheep, pig, camel and deer skin in colla corii asini by ultra performance liquid chromatography-tandem mass spectrometry

HANG Baojian1, TIAN Chenying2, CHEN Xiao1, XING Sheng1, SHI Feng1, LENG Jiawei1, GONG Liping1   

  1. 1. Shandong Institute for Food and Drug Control, Jinan 250101, China;
    2. Shandong University of Traditional Chinese Medicine, Jinan 250355, China
  • Received:2017-11-03 Online:2018-04-08 Published:2014-02-26
  • Supported by:

    Major New Drug Creation Program of China (No. 2014ZX0930437).

摘要:

建立了阿胶中马、牛、羊、猪、骆驼、鹿皮源成分的检测方法。通过比对驴皮和马皮、牛皮、猪皮、羊皮、骆驼皮、鹿皮胶原蛋白的序列,采用蛋白酶切技术和高分辨质谱技术发现理论的各杂皮胶原蛋白特征肽。同时建立三重四极杆质谱筛查方法,以含0.1%(v/v)甲酸的乙腈溶液和0.1%(v/v)甲酸水溶液作为流动相,梯度洗脱,电喷雾离子源(ESI)正离子扫描模式,多反应监测。15批阿胶样品检出了杂皮源成分。该方法操作简便,专属性强,可用于阿胶中杂皮源成分的鉴别,并已成功用于阿胶日常打假监督抽验工作。

关键词: 阿胶, 超高效液相色谱-串联质谱, 胶原蛋白, 特征肽

Abstract:

A method was established for detecting the ingredients of horse, ox, sheep, pig, camel and deer skin in colla corii asini using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).Theoretical marker peptides were selected by comparing the collagen sequences in the skins of donkeys, horses, oxen, sheep, pigs, camels, and deer.Marker peptides were identified by protease cutting techniques and high resolution mass spectrometry and then analyzed by UPLC-MS/MS.The separation was performed on a UPLC system with a BEH C18 column via the gradient elution of acetonitrile containing 0.1%(v/v) acetic acid and water containing 0.1%(v/v) acetic acid.The marker peptides were identified in the modes of electrospray positive ionization (ESI+) and multiple reaction monitoring (MRM).The marker peptides for the horse, ox, sheep, pig and camel skin were detected in 15 samples.The method is simple, highly reproducible, and suitable for the identification of mixed skin ingredients in colla corii asini.It has been successfully used to detect the authenticity of colla corii asini.

Key words: colla corii asini, collagen, marker peptide, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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