陈欣慰 屠雨晨 黄芳 汤逸飞 张国平

摘 要：为明确生产的柑橘中的农药残留情况，以嘉兴市为例，采用QuEChERS前处理、气相色谱分离、多反应监测（MRM）和外标法定量等方式对样品进行分析，并通过慢性膳食摄入风险评估进行评价。34种农药在50～250 μg/L的范围内线性关系良好，回归方程相关系数（r2）在0.994 0～0.999 5，添加回收率（P）在61.27%～121.80%，相对标准偏差（RSD）在0.06%～11.62%。結果未发现禁用农药，检出农药按照国家标准或慢性膳食摄入风险评估均未超限。柑橘中毒死蜱残留检出频次较多，要注意毒死蜱残留指标可能日趋严格。

关键词：柑橘;农药残留;气相色谱三重四级杆串联质谱法

文章编号：2096-8108（2021）06-0027-04  中图分类号：S481+.8  文献标识码：A

Chemical Screening and Determination of 34 Kinds of Pesticide Residues in Citrus

CHEN Xinwei，TU Yuchen，HUANG Fang，TANG Yifei，ZHANG Guoping*

（Jiaxing Center for Inspection and Testing of Agriculture， Jiaxing 314000， China）

Abstract：In view of pesticide residues in citrus planting， a sample pretreatment method coupled with GC-MS/MS was established to determine 34 pesticide residues.The target compounds were detected by electron impact ionization in MRMmode with external standard method and the detected data wereperformed with chronicrisk assessment （%ADI）. The test results showed that the method appeared to be a good linear relationship for 34 pesticides in theconcentration ranges of 50～250 μg/L， with the correlation coefficient

（r2）of 0.994 0～0.999 5. Moreover， the average recoverieswere in the range of 61.27%～121.80% with RSD between0.06% and 11.62%. The procedure for citrus could be used for rapid screening and determination of 34 pesticides and it proved to be relativly safe incitrus plantingon 34 pesticide residues. The chlorpyrifos residue indicatorin citrus should be stricter due to the detection frequency of chlorpyrifos residuesyet.

Keywords：citrus; pesticide residues; GC-MS/MS

柑橘属于芸香科柑桔属，早在2300年前，包括嘉兴的浙江北部一带已经有柑橘记载[1]。柑橘果实成熟期约在每年的10月-12月，因果实汁水充足，酸甜可口，深受广大消费者的喜爱。为保证果实有“卖相”[2]，化学类农药的喷施不可缺少。因施药频率较高会给橘产品带来一定的质量安全风险，可能使消费者在食用时因农药残留超标而带来健康隐患。根据农药残留水平分析，筛查柑橘中常用禁限用农药及杀虫剂的残留水平并评价其风险状况，以嘉兴市为例，通过检测明确柑橘中主要的农药残留种类以及需重点关注的农药风险因子，为柑橘产品安全生产、消费及质量安全监管提供一定的借鉴和依据。

1 样品、仪器和试剂

样品来源于嘉兴地区18家家庭农场，对应采集样品18批次，其中柑橘常见品种“宫川”15批次、新引进品种“红美人”3批次，每份样品质量不少于2 kg。……