摘要
建立了芹菜中甲拌磷及其代谢物（甲拌磷亚砜和甲拌磷砜）残留的液相色谱/串联质谱检测方法。样品以乙腈提取,采用电喷雾正离子源（ESI＋）和多重反应监测（MRM）模式测定,基质匹配标准曲线定量。结果表明：芹菜基质中甲拌磷、甲拌磷亚砜和甲拌磷砜在0.01-0.1mg/L范围内线性关系均较好（r〉0.995）,方法检出限和定量限分别为0.42-1.10μg/kg和1.4-3.6μg/kg;在5、50和100μg/kg三个添加水平下,甲拌磷、甲拌磷亚砜和甲拌磷砜的回收率为71.9%-90.2%,相对标准偏差为5.8%-9.9%。该法简单、准确、快速、灵敏,符合法规残留限量监测要求。
A method was established for the determination of phorate and its metabolites（phorate sulfoxide and phorate sulfone）residues in celery by liquid chromatography/tandem mass spectrometry.The test sample was extracted with acetonitrile.Electrospray positive ion source（ESI＋）,multiple reaction monitoring mode（MRM）and matrix-matched external standard method were applied for sample analysis.The calibration curves showed good linearity within the range of 0.01-0.1 mg/L with correlation coefficient（r）larger than 0.995 in celery,the limits of detection and limits of quantification were 0.42-1.10μg/kg and 1.4-3.6μg/kg,respectively.The method validation was carried out at three spiked levels of 5,50,100μg/kg.The recoveries were from 71.9% to 90.2%,and the RSDs were from5.8% to 9.9%.The method is sensitive and suitable for monitoring of the maximum residue limits（MRLs）of phorate,phorate sulfoxide and phorate sulfone.
出处
《分析科学学报》
CAS
CSCD
北大核心
2016年第2期294-296,共3页
Journal of Analytical Science
关键词
液相色谱/串联质谱
甲拌磷
芹菜
Liquid chromatography/tandem mass spectrometry
Phorate
Celery
作者简介
吴成，男，博士，高级农艺师，主要从事农药残留分析研究．E—mail：wucheng7745@sina．com
