液相色谱串联质谱法测定谷物类农产品中苯氧羧酸类除草剂多残留  

Determination of Multi-residues of Phenoxy Acid Herbicides in Cereals by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：程静[1,2] 丁磊[2] 蒋俊树[1,2] 卢业举[1,2] 

机构地区：[1]安徽国家农业标准化与监测中心,安徽合肥230051 [2]安徽大学化学化工学院,安徽合肥230039

出　　处：《食品科学》2010年第20期389-393,共5页Food Science

基　　金：国家质检公益性行业科研专项(200810773)

摘　　要：研究液相色谱-串联质谱(LC-ESI-MS/MS)测定大米、小麦、玉米等谷物中6种苯氧羧酸类除草剂(2,4-DP、2,4-D、2,4,5-TP、2,4,5-T、2,4-DB、MCPA)残留量的方法。通过对样品前处理进行优化研究,样品经乙腈提取,乙酸酸化,净化后,采用HPLC-ESI-MS/MS检测分析,在多反应监测模式(MRM)下,外标法定量。方法的检出限为0.005～0.01mg/kg,在0.01～0.5mg/L范围内线性关系良好(相关系数r2>0.99),在0.2mg/kg添加水平下,平均添加回收率86.1%～96.8%,该方法简便、高效、准确,各项技术指标均满足国内外有关苯氧羧酸类除草剂残留限量要求,可用于大米、小麦、大豆等农产品中苯氧羧酸类除草剂残留的分析测定。A new method using liquid chromatography-electrospray ionization tandem mass spectrometry （LC-ESI-MS/MS） for the analysis of six phenoxy acid herbicide residues in cereals has been developed. The optimized sample pretreatment procedure consisted of extraction with acetonitrile,acidification with acetic acid and cleanup before the analysis on a LC-ESI-MS/MS instrument. Separated analytes were determined using multiple reaction monitoring （MRM）. Quantitation was per-formed using external standard method. The proposed method displayed a detection limit between 0.005 and 0.01 mg/kg and good linearity over the range from 0.01 to 0.5 mg/L,with a r2 0.99. At a spike level of 0.2 mg/kg,mean recoveries from rice ranged between 86.1% and 96.8% for different analytes. The method is simple,efficient and sensitive,and its each performance characteristic meets the requirements for the determination of phenoxy acid herbicide residues in cereasl at home and abroad.

关 键 词：苯氧羧酸类除草剂 谷物 高效液相色谱-串联质谱 

分 类 号：TS207.53[轻工技术与工程—食品科学]