QuEChERS-气相色谱-质谱法测定土豆中109种农药残留  

Determination of 109 pesticide residues in potato using QuEChERS clean-up and gas chromatography-mass spectrometry

作　　者：吕冰[1] 朱盼[1] 李荷丽[1] 杜晓林[1] 赵云峰[1] 苗虹[1] 

机构地区：[1]国家食品安全风险评估中心卫生部食品安全风险评估重点实验室,北京100021

出　　处：《中国食品卫生杂志》2014年第3期238-244,共7页Chinese Journal of Food Hygiene

基　　金：国家科技支撑计划(2011BAK10B06)

摘　　要：目的 建立土豆中109种农药残留的气相色谱-质谱（GC-MS）检测方法。方法 土豆样品以乙腈提取后,经N-丙基乙二胺（PSA）分散固相萃取净化（d-SPE）,采用电子轰击电离源（EI）和负化学电离源（NCI）两种电离模式进行GC-MS测定。结果 各农药的定量限在0.001～0.010mg/kg之间,对空白土豆样品的平均加标回收率为72.7%～118.7%,RSD在1.1%～17.3%之间。在EI模式下,土豆基质对绝大多数农药具有明显的基质效应,因此采用基质匹配标准曲线进行定量分析。应用此方法对欧盟农药残留参比实验室组织的国际比对考核的土豆样品进行定性筛查和定量测定,共检测出13种农药残留,含量范围在0.002～1.669mg/kg之间,所提交的测定结果的Z评分值在-1.00～1.00之间。结论 本方法简便快速、准确、灵敏度高,适用于农产品中农药多残留的分析。Objective A modified QuEChERS method for simultaneous determination of 109pesticide residues in potato using gas chromatography coupled with mass spectrometry was established and validated.MethodsThe pesticide residues were extracted from the potato samples with acetonitrile, and purified by dispersion solid phase extraction （d-SPE） using N-propyl ethlene diamine （PSA） as the adsorbent. The GC-MS analysis was carried out under selected ion monitoring mode and the quantification was performed using the external standard calibration. ResultsThe limits of quantification （LOQ） for 109pesticide were in the range of 0.001-0.010mg/kg. The recoveries were between 72.7% and 118.7% with the RSD of 1.1%-17.3%. When using electron impact （EI） mode, most pesticides exhibited matrix enhancement effects in potato matrix. To ensure an accurate determination, the matrix-matched calibration was used for quantitation. The established method was successfully applied to the potato samples provided by European proficiency test in fruits and vegetables organized by European Union Reference Laboratory for Residues of Pesticides in Fruits and Vegetables, and 13pesticides were detected with the concentration in the range of 0.002-1.669mg/kg with the Z-scores in the range of -1.00 to 1.00.ConclusionThe method was simple, sensitive, accurate and suitable for the fast screening test for multi-residue pesticides in potato.

关 键 词：QUECHERS 气相色谱-质谱法 农药残留 土豆 基质效应 

分 类 号：O657.63[理学—分析化学] TS207.53[理学—化学]