色谱

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免疫亲和萃取-超高效液相色谱-串联质谱法分离测定中成药及中药材中的5种黄曲霉毒素

韩深1, 刘萤1, 吕美玲2, 李建中2, 王金花1*   

  1. 1. 北京出入境检验检疫局技术中心, 北京 100026; 2. 安捷伦科技(中国)有限公司, 北京 100102
  • 收稿日期:2011-04-14 修回日期:2011-05-17 出版日期:2011-07-28 发布日期:2011-08-19
  • 通讯作者: 王金花,博士,高级工程师. Tel: (010)58619247,
  • 基金资助:

    北京市科委计划项目(D0805020031085)

Recent applications of solid-phase extraction techniques for analysis of trace residues and contaminants in food

HAN Shen1, LIU Ying1, L, Meiling2, LI Jianzhong2, WANG Jinhua1*   

  1. 1. Technical Centre of Beijing Entry-Exit Inspection and Quarantine Bureau, Beijing 100026, China; 2. Agilent Technologies (China) Co., Ltd., Beijing 100102, China
  • Received:2011-04-14 Revised:2011-05-17 Online:2011-07-28 Published:2011-08-19

摘要: 利用免疫亲和萃取结合超高效液相色谱-串联四极杆质谱技术(UHPLC-ESI/QqQ-MS/MS)建立了中成药及中药材中5种黄曲霉毒素(B1、B2、G1、G2和M1)的提取、分离、确证与定量方法。样品经80%(体积分数)的甲醇水溶液提取和免疫亲和固相萃取后,采用UHPLC-ESI/QqQ-MS/MS的多反应监测模式实现分离、鉴定和外标法定量。5种目标毒素标准溶液的检出限(LOD)为0.05~0.3 μg/L。在0.5~100 μg/L的基质添加浓度范围内具有良好的线性关系(r2>0.99);以甘草为例,当添加水平为1.0 μg/kg和5.0 μg/kg时,得到62.3%~82.4%的回收率(相对标准偏差(RSD)<10%, n=6)。该方法灵敏度高、选择性和重复性好、回收率较高、检测速度快,适用于中成药及中药材等复杂基体中多种黄曲霉毒素的快速分析与筛查。

关键词: 超高效液相色谱-串联质谱, 黄曲霉毒素, 免疫亲和萃取, 中成药, 中药材

Abstract: The determination of trace residues and contaminants in food often requires extensive sample extraction and preparation prior to instrumental analysis. Due to the multiplicity and complexity of food matrices, it is not possible to use only one sample preparation technique. This review introduces the application of some new techniques of solid-phase extraction (SPE) in recent years, such as solid-phase microextraction (SPME), stir-bar sorptive extraction (SBSE), matrix solid-phase dispersion (MSPD), molecularly imprinted solid-phase extraction (MISPE), immunoaffinity-based solid-phase extraction (IASPE), monolithic solid-phase extraction, carbon nanotube solid-phase extraction, in the analysis of trace residues and contaminants in food. At last, future developments in this field are outlined.

Key words: carbon nanotube solid-phase extraction, food analysis, immunoaffinity-based solid-phase extraction (IASPE), monolithic solid-phase extraction, matrix solid-phase dispersion (MSPD), molecularly imprinted solid-phase extraction (MISPE), solid-phase microextraction (SPME), stir-bar sorptive extraction (SBSE)