色谱

色谱 ›› 2012, Vol. 30 ›› Issue (03): 314-318.DOI: 10.3724/SP.J.1123.2011.11018

• 技术与应用 • 上一篇    下一篇

高效液相色谱-串联质谱法测定蜂胶中的氯霉素

张晓燕*, 张睿, 许蔚, 黄娟, 刘艳, 吴斌, 陈磊, 丁涛, 沈崇钰, 陈惠兰   

  1. 江苏出入境检验检疫局动植物与食品检测中心 国家蜂产品基准实验室, 江苏 南京 210001
  • 收稿日期:2011-11-11 修回日期:2011-12-16 出版日期:2012-03-28 发布日期:2012-05-02
  • 通讯作者: 张晓燕,硕士研究生,工程师. Tel: (025)52345187
  • 基金资助:

    国家质量监督检验检疫总局科技项目(2012IK167).

Determination of chloramphenicol in propolis by high performance liquid chromatography- tandem mass spectrometry

ZHANG Xiaoyan*, ZHANG Rui, XU Wei, HUANG Juan, LIU Yan, WU Bin, CHEN Lei, DING Tao, SHEN Chongyu, CHEN Huilan   

  1. National Honey Reference Laboratory, Animal, Plant and Food Inspection Center (APFIC) of Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China
  • Received:2011-11-11 Revised:2011-12-16 Online:2012-03-28 Published:2012-05-02

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摘要：

建立了高效液相色谱-串联质谱(HPLC-MS/MS)测定蜂胶中氯霉素残留的方法。样品用水提取后,以醋酸铅溶液作为沉淀剂除去样品中的大部分黄酮类成分,用液-液萃取的方式提取样品中的氯霉素残留,最后以HPLC-MS/MS对样品进行定性、定量分析。该方法采用内标法定量,线性范围为0.05～2.0 μg/L,相关系数为0.9996;方法的检出限(以信噪比(S/N)为3计)和定量限(以S/N=10计)分别为0.1 μg/kg和0.3 μg/kg;回收率范围为70.1%～94.0%,日内精密度小于10%,日间精密度在15.0%以下。该方法简便快捷,能除去蜂胶中的大部分黄酮类成分,减少了干扰,可以用于蜂胶中氯霉素残留的测定。

关键词: 蜂胶, 高效液相色谱-串联质谱, 氯霉素

Abstract:

A method for the determination of chloramphenicol in propolis was developed by high performance liquid chromatography-tandem mass spectrometry. The flavones were removed with lead acetate solution after the extraction of the sample with water. The extract was cleaned up by liquid-liquid extraction. Internal standard method was used for quantitative analysis. The linear range was 0.05~2.0 μg/L and the correlation coefficient (r2) was 0.9996. The limit of detection (LOD, S/N=3) and limit of quantitation (LOQ, S/N=10) were 0.1 μg/kg and 0.3 μg/kg, respectively. The recoveries ranged from 70.1% to 94.0% while the intra-day precision lower than 10% and inter-day precision lower than 15%. The method reduced the interference by removing most of the flavones and was suitable for the determination of chloramphenicol in propolis.

Key words: chloramphenicol, propolis, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)