色谱

色谱 ›› 2018, Vol. 36 ›› Issue (7): 643-650.DOI: 10.3724/SP.J.1123.2018.01041

• 研究论文 • 上一篇    下一篇

超高效液相色谱-线性离子阱/静电场轨道阱质谱法快速检测化妆品中66种抗生素

李红英1, 沈华旦2, 方江济3, 张静雅1, 丁晓萍1   

  1. 1. 湖北省药品监督检验研究院, 湖北 武汉 430075;
    2. 湖北中医药大学药学院, 湖北 武汉 430065;
    3. 武汉理工大学化学化工与生命科学学院, 湖北 武汉 430070
  • 收稿日期:2018-01-25 出版日期:2018-07-08 发布日期:2014-06-03
  • 通讯作者: 丁晓萍,Tel:027,87705274,E-mail:dxp2888@126.com

Rapid determination of 66 antibiotics in cosmetics using ultra high performance liquid chromatography-linear ion trap/Orbitrap mass spectrometry

LI Hongying1, SHEN Huadan2, FANG Jiangji3, ZHANG Jingya1, DING Xiaoping1   

  1. 1. Hubei Institute for Drug Control, Wuhan 430075, China;
    2. School of Pharmaceutical Science, Hubei University of Chinese Medicine, Wuhan 430065, China;
    3. School of Chemistry, Chemical Engineering and Life Sciences, Wuhan University of Technology, Wuhan 430070, China
  • Received:2018-01-25 Online:2018-07-08 Published:2014-06-03

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摘要：

采用超高效液相色谱-线性离子阱/静电场轨道阱高分辨质谱法同时测定化妆品中磺胺类、沙星类等66种抗生素类化合物，建立了快速筛查数据库和定量分析方法。待测物用乙腈超声提取，C18色谱柱（100 mm×2.1 mm，1.8 μm）分离，以0.1%（v/v）甲酸水溶液和乙腈为流动相进行梯度洗脱。在正离子模式下，以保留时间和一级母离子精确质量数进行快速筛查，以高能碰撞诱导解离获得的二级碎片离子精确质量数进行确证。结果表明，化合物的线性关系良好，线性相关系数（R2）>0.99；检出限（LOD）为2~4 μg/kg；定量限（LOQ）为5~10 μg/kg；3个添加水平（1LOQ、10LOQ、30LOQ）的平均回收率为58.2%~119.1%，相对标准偏差为1.03~11.9%。该方法简便快速、定性定量可靠，适用于化妆品中抗生素类化合物的快速筛查和定量检测。

关键词: 超高效液相色谱, 化妆品, 抗生素, 线性离子阱/静电场轨道阱高分辨质谱法

Abstract:

A rapid screening and determination method, in conjunction with a database for confirmation, was established based on 66 antibiotic compounds using ultra-high performance liquid chromatography-linear ion trap/Orbitrap high resolution mass spectrometry (UPLC-LTQ/Orbitrap MS). The analytes were extracted with acetonitrile using ultrasonic extraction. The separation was performed on a C18 column (100 mm×2.1 mm, 1.8 μm) with a gradient elution of 0.1% (v/v) formic acid and acetonitrile. The retention time and accurate mass of the precursor ion were used for rapid screening in positive ionization mode, with the fragment ions obtained by higher energy collisional dissociation used for confirmation. The results indicated that each compound showed good linearity with a correlation coefficient of R2>0.99. The limits of detection (LODs) were in the range 2-4 μg/kg, and the limits of quantification (LOQs) were in the range 5-10 μg/kg. The average recoveries at three levels (1LOQ, 10LOQ, and 30LOQ) were between 58.2% and 119.1%, and the relative standard deviations (RSDs) were between 1.03% and 11.9%. The method is simple, rapid, reliable, and accurate, which is suitable for rapid screening and determination of the 66 antibiotic compounds in cosmetics.

Key words: antibiotics, cosmetics, linear ion trap/Orbitrap high resolution mass spectrometry(LTQ/Orbitrap MS), ultra-high performance liquid chromatography(UPLC)

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