高效液相色谱-电喷雾串联质谱法快速测定纺织品中苯氧羧酸类除草剂残留量  

Rapid Determination of Phenoxy Acid Herbicide Residues in Textiles by Liquid Chromatography-Electrospray Ionization Tandem Mass Spectrometry

作　　者：牛增元[1] 罗忻[1] 汤志旭[1] 叶曦雯[1] 孙银峰[2] 张鸿伟[1] 王凤美[1] 

机构地区：[1]山东出入境检验检疫局生态纺织品检测国家级重点实验室,青岛266002 [2]青岛科技大学环境与安全工程学院,青岛266042

出　　处：《分析化学》2009年第4期505-510,共6页Chinese Journal of Analytical Chemistry

基　　金：质检公益性行业科研专项经费(No.10-66);国家认证认可监督委员会标准制订(No.2005B124)资助项目

摘　　要：建立了纺织品中7种苯氧羧酸类除草剂的高效液相色谱-电喷雾串联质谱(LC-ESI-MS/MS)快速检测方法。样品经甲酸酸化的丙酮溶液超声提取两次,无需其它净化过程。液相色谱使用C18反相色谱柱,流动相为醋酸铵水溶液和甲醇,在梯度条件下分析。在选择反应检测(SRM)负离子模式下进行质谱信号采集,采用两对同位素离子对进行定性和定量分析。选取3种有代表性的纺织品进行方法检出限(LOD)、定量限(LOQ)、线性、回收率和精密度的验证。方法的LOQ为0.9～2.4μg/kg;回收率为85%～106%;相对标准偏差为2%～11%。本方法简便、有效、可靠、灵敏,能够满足国际生态纺织品标准(Oeko-Tex Standard 100)的限量要求,适用于纺织品中苯氧羧酸类除草剂的日常检测及确证。A simple and efficient method for rapid determination of 7 phenoxy acid herbicide residues in textiles, based on the use of liquid chromatography electrospray ionization tandem mass spectrometry （ LC-ESIMS/MS） , is reported. Sample treatment procedure entailing the use of twice ultrasonic extraction steps with acetone（acidified by formic acid） without any clean-up was developed. A reversed-phase C18 column with an aqueous ammonium acetate/methanol mixture as the mobile phase was used under gradient elution. Mass spectral acquisition was done in negative ion mode by applying selected reaction monitoring（SRM）. Two isotopic fragmentation transitions per compound were used to provide a high degree of selectivity. The method was in-house validated in terms of limit of detections（LODs） , limit of quantitations（LOQs）, linearity, recovery, precision on three typical kinds of textiles. Good results in the low μg/kg level were obtained for LODs and LOQs of all analytes in matrices. Extraction recoveries for 7 phenoxy acid herbicides ranged from 85% to 106% and RSD was between 2% - 11%. The method fulfils Oeko-Tex Standard 100 demands for routine monitoring and verification of phenoxy acid herbicides.

关 键 词：高效液相色谱-电喷雾串联质谱 除草剂残留 苯氧羧酸 纺织品 

分 类 号：TS101.9[轻工技术与工程—纺织工程]