一种新型固相萃取柱结合超高效液相色谱-串联质谱法选择性富集测定猪肉中的盐酸克伦特罗  

A novel solid phase extraction column combined with ultra performance liquid chromatography/tandem mass spectrometry for selective enrichment and determination of clenbuterol in pork

作　　者：孟文瑛[1] 郭志谋[2] 沈伟健[3] 沈崇钰[3] 吴斌[3] 刘艳明[4] 章飞芳[1] 梁鑫淼[1,2] 

机构地区：[1]华东理工大学药学院,上海200237 [2]中国科学院大连化学物理研究所,辽宁大连116023 [3]江苏出入境检验检疫局食品实验室,江苏南京210001 [4]山东省产品质量监督检验研究院,山东济南250103

出　　处：《色谱》2012年第2期141-145,共5页Chinese Journal of Chromatography

基　　金：国家科技支撑计划项目(No.2009BADB9B02);国家自然科学基金项目(No.21177040);上海市科委重点基础研究项目(No.09JC1403900)

摘　　要：发展了一种测定猪肉中盐酸克伦特罗残留的简便、高效、准确的固相萃取-超高效液相色谱-串联质谱(SPE-UPLC-MS/MS)的方法。将搅碎的猪肉样品用5%(v/v)高氯酸超声提取,再以10 000 r/min离心15 min后,上清液用SMCX固相萃取柱进行富集和净化。因SMCX是以硅胶为基质兼有反相/强阳离子交换的混合作用模式,因此可以有效地去除复杂基质干扰,达到目标样品的选择性富集和净化的目的。方法学结果表明,该方法在0.25～50μg/kg范围内具有良好的线性关系,相关系数r为0.998 2;3个添加水平(1.25、12.5、50μg/kg)的平均回收率为62.2%～72.0%,相对标准偏差(RSDs)为4.2%～6.1%;检出限(S/N=3)为0.05μg/kg。所发展的样品前处理和检测方法简单、快速,可用于瘦肉精类成分的选择性富集和分离检测。A simple and efficient method based on a novel solid phase extraction（SPE） cartridge and ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） was developed for the determination of clenbuterol residue in pork.The minced pork sample was ultrasonically extracted by 5%（v/v） perchloric acid and centrifuged at 10 000 r/min for 15 min,then the supernatant was purified by an SMCX cartridge,which is a novel SPE column based on homemade silica matrix with two mixed modes of reversed-phase and strong cation exchange,for the selective enrichment and purification of the analyte.The linear range of the method was 0.25-50 μg/kg with a correlation coefficient of 0.998 2.The average recoveries ranged from 62.2% to 72.0% at the three spiked levels of 1.25,12.5 and 50 μg/kg with the relative standard deviations（RSDs） between 4.2% and 6.1%.The limit of detection（S/N=3） was 0.05 μg/kg.The method is simple,fast and can be extended to enrich and determine β-agonist drugs.

关 键 词：固相萃取 超高效液相色谱-串联质谱 SMCX柱 盐酸克伦特罗 猪肉 

分 类 号：O658[理学—分析化学]