液相色谱-串联质谱法快速测定粮谷中的矮壮素和敌草快残留量.docVIP

液相色谱-串联质谱法快速测定粮谷中的矮壮素和敌草快残留量 曹 慧(，陈小珍，张东雷，祝 颖，武晓光 ( 浙江省质量检测科学研究院 食品检测部，杭州 310013 ) 摘要：采用液相色谱-串联质谱技术（UPLC/MS/MS）快速分析粮谷中的矮壮素和敌草快残留量。样品经甲醇-水-乙酸溶液提取，HLB固相萃取小柱净化，用液相色谱-串联质谱法测定，外标法定量。结果表明，矮壮素和敌草快在5～50μg/L范围内线性关系良好；矮壮素的加标回收率在77.7%~93.1%之间，敌草快的加标回收率在73.9%~95.3%之间；两者相对标准偏差均小于15%；矮壮素和敌草快的检出限分别为2.5μg/kg和5.0μg/kg，定量下限分别为10μg/kg和20μg/kg。该方法完全满足粮谷中矮壮素和敌草快残留量的快速分析。 关键词：液相色谱-串联质谱；敌草快；矮壮素；粮谷 中图分类号： O657.63 文献标识码：A 文章编号： Determination of the Residues of Chlormequat and Diquat in Grains Using Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry CAO Hui, CHEN Xiao-zhen, ZHANG Dong-lei, ZHU Ying, WU Xiao-guang, ( Zhejiang Institute of Quality Inspection Science, Hangzhou 310013, China ) Abstract: A method was developed for determination of the residues of chlormequat and diquat in grains using ultra performance liquid chromatography-tandem mass spectrometry (UPLC/MS/MS). The samples were extracted with methanol-water-acetic acid solution, passed through HLB cartridge to clear-up and determined by UPLC/MS/MS using external standard method. The linear range was 5μg/L ~50μg/L and the correlation coefficient (r2) was more than 0.998. The average recoveries were in the range from 77.7% to 93.1% for chlormequat. The average recoveries ranged from 73.9% to 95.3% for diquat. The relative standard deviation (RSD) were less than 15%. The limit of detection (LOD) were 2.5 μg/kg and 5.0 μg/kg in chlormequat and diquat, and the limit of quantitation (LOQ) were 10 μg/kg and 20 μg/kg respectively. The simplicity, sensitivity and good precision of the method made it be well suitable for the analysis of chlormequant and diquat in grains. Keywords: ultra performance liquid chromatography-tandem mass spectrometry; chlormequat; diquat; grains 矮壮素和敌草快是一类季铵盐类化合物，矮壮素又称稻麦立，化学名为2-氯乙基三甲铵氯化物，是一种植物生长调节剂，可抑制植物体赤霉素的合成、促进植物生殖生长、提高作物产品质量和品质，广泛用于小麦、水稻和棉花等农作物[1-3]。敌草快是一种广谱性除草剂，能被叶片吸收，抑制光合作用，破坏细胞膜，使之枯黄。该农药不仅在土壤中残留活性仅几天，而且对阔叶杂草效果更好，因而，适用于非耕地、免耕地播前除草，果园、作物行间除草，也可用于大豆、棉花等作物收获前的催枯脱叶。日本