色谱

色谱

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同位素稀释液相色谱-串联质谱法准确测定猪肉中的氯霉素

杨总, 李秀琴, 王娟, 张庆合*   

  1. 中国计量科学研究院, 北京 100013
  • 收稿日期:2011-08-01 修回日期:2011-08-19 出版日期:2011-09-28 发布日期:2011-10-28
  • 通讯作者: 张庆合,博士,研究员,研究方向为仪器分析技术与方法. Tel: (010)64228593
  • 基金资助:

    国家科技基础性工作专项项目(2008FYl30200).

Accurate determination of chloramphenicol in pork by isotope dilution liquid chromatography-electrospray ionization tandem mass spectrometry

YANG Zong, LI Xiuqin, WANG Juan, ZHANG Qinghe*   

  1. National Institute of Metrology, Beijing 100013, China
  • Received:2011-08-01 Revised:2011-08-19 Online:2011-09-28 Published:2011-10-28

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摘要： 建立了同位素稀释质谱测定猪肉中氯霉素残留的方法,对影响溶剂提取、萃取净化、液相色谱-质谱检测方法准确度的因素进行了量化与优化。猪肉样品经液氮冷冻粉碎,加入氯霉素-D5同位素内标和0.1 mol/L醋酸钠缓冲溶液(pH 5),用乙酸乙酯提取4次,正己烷脱脂,HLB固相萃取小柱净化后采用负离子多反应监测模式下的液相色谱-质谱技术检测。方法的线性范围为0.01～0.5 ng/g,相关系数r2大于0.999;检出限和定量限分别为0.004 ng/g和0.02 ng/g;在0.02 ng/g和1.0 ng/g加标水平的回收率(n=3)分别为95.2%～109.1%和99.7%～102.5%;日内和日间相对标准偏差均小于2%。研究了氯霉素及氯霉素-D5的基体效应,测得不同流动相和稀释溶剂组成时基体效应因子k的范围在0.950～1.015之间。研究结果对同位素稀释质谱痕量残留检测结果准确度的控制、方法的建立与验证具有参考意义。

关键词: 基体效应, 氯霉素, 同位素稀释, 液相色谱-电喷雾串联质谱法, 猪肉

Abstract: An accurate method was described for the determination of chloramphenicol (CAP) in pork. The analyte was quantified by isotope dilution liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) operating in negative ion multiple reaction monitoring (MRM) mode. The sample was treated by liquid-liquid extraction with ethyl acetate followed by a clean-up step on an HLB solid-phase extraction cartridge. Chloramphenicol-D5 (CAP-D5) was added as an isotope internal standard. Under the optimized conditions, the calibration curve showed a good linearity in ranging from 0.01 to 0.5 ng/g CAP. The correlation coefficient r2 was 0.9998. The limit of detection and the limit of quantification were 0.004 and 0.02 ng/g, respectively. The average recoveries of CAP at 0.02 ng/g and 1.0 ng/g spiked levels ranged from 95.2%~109.1%, 99.7%~102.5%, respectively. The relative standard deviations (RSDs) of intra-day and inter-day were less than 2%. Meanwhile, matrix effect factors k of CAP and CAP-D5 were determined under different mobile phases and the sample solvent composition, the k was in the range of 0.950~1.015. The method can be used as a confirmed method for the determination of CAP in pork.

Key words: chloramphenicol, liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS), matrix effect, pork, isotope dilution