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日用化学工业 ›› 2014, Vol. 44 ›› Issue (7): 406-409.doi: 10.13218/j.cnki.csdc.2014.07.091

• 分析与检测 • 上一篇    下一篇

液相色谱-四极杆/离子阱串联质谱法测定牙膏中的绿原酸

马晓斐1, 宋炜2, 梁天佐1, 贾振国1, 冯浩彬1, 张岩1   

  1. 1.河北省食品质量监督检验研究院,河北 石家庄 050091;
    2.河北省食品药品检验院,河北 石家庄 050011
  • 收稿日期:2014-02-19 出版日期:2014-07-22 发布日期:2019-04-08
  • 通讯作者: 张 岩,高级工程师,E-mail:snowwinglv@126.com。
  • 作者简介:马晓斐(1984-),男,河北人,工程师,E-mail:xiaofeima1984@163.com。

Detection of chlorogenic acid in toothpaste by liquid chromatography coupled to quadrupole/linear ion trap tandem mass spectrometry

MA Xiao-fei1, SONG Wei2, LIANG Tian-zuo1, JIA Zhen-guo1, FENG Hao-bin1, ZHANG Yan1   

  1. 1.Hebei Institute of Food Quality Supervision Inspection and Research,Shijiazhuang,Hebei 050091,China;
    2.Hebei Provincial Institute for Food and Drug Control,Shijiazhuang,Hebei 050011,China
  • Received:2014-02-19 Online:2014-07-22 Published:2019-04-08

摘要: 建立了液相色谱-四极杆/离子阱串联质谱(LC-QTRAP-MS/MS)测定牙膏中绿原酸的方法。试样经超声提取,Kinetex C18色谱柱(2.1 mm×100 mm,2.6 μm)分离,以甲醇-0.1%甲酸水溶液为流动相洗脱,采用多反应监测(MRM)-信息依赖性采集(IDA)-增强子离子扫描(EPI)模式检测,外标法定量。结果表明,绿原酸在质量浓度为1.0~100 μg·L-1范围内线性关系良好(r=0.999 6),方法检出限为10.0 μg·kg-1,在低、中、高3个添加水平时的平均回收率为85.6%~96.6%,相对标准偏差均不大于5.8%。

关键词: 牙膏, 液相色谱, 四极杆/离子阱串联质谱, 绿原酸

Abstract: A comprehensive method for detection of chlorogenic acid in toothpaste was established with liquid chromatography coupled to quadrupole/linear ion trap tandem mass spectrometry (LC-QTRAP-MS/MS).The samples were extracted under ultrasonic assistance.The separation was carried out on a Kinetex C 18 column (2.1 mm×100 mm,2.6 μm) using mobile phases of methanol-0.1% formic acid solution as eluant.A multiple reaction monitoring (MRM) in negative mode as survey scan and an enhanced production (EPI) scan as dependent scan in an information-dependent acquisition (IDA) experiment was adopted in mass spectrometry acquisition.External standard was employed for the quantification.Test results showed that content of the chlorogenic acid displays good linearity within 1.0~100 μg·L-1 vs.the peak area of the chromatogram with a correlation coefficient (r) of 0.999 6.The limit of detection for the chlorogenic acid is 10.0 μg·kg-1.The mean recoveries at the three spiked levels are 85.6%~96.6%,and the relative standard deviations are not higher than 5.8%.

Key words: toothpaste, liquid chromatography, quadrupole/linear ion trap tandem mass spectrometry, chlorogenic acid

中图分类号: 

  • TQ658.4