中成药2024,Vol.46Issue(1) :143-149.DOI:10.3969/j.issn.1001-1528.2024.01.025

GC-MS法同时测定枸杞中16种农药残留的含量及安全性评价

Simultaneous GC-MS determination of sixteen pesticide residues and safety assessment for Lycii Fructus

秦佳琪 齐强强 张亚军 王焱 赵思源 曹德艳 朱美霖
中成药2024,Vol.46Issue(1) :143-149.DOI:10.3969/j.issn.1001-1528.2024.01.025

GC-MS法同时测定枸杞中16种农药残留的含量及安全性评价

Simultaneous GC-MS determination of sixteen pesticide residues and safety assessment for Lycii Fructus

秦佳琪 1齐强强 2张亚军 2王焱 1赵思源 1曹德艳 1朱美霖3
扫码查看

作者信息

  • 1. 宁夏医科大学公共卫生与管理学院, 宁夏 银川 750004;宁夏医科大学, 宁夏环境因素与慢性病控制重点实验室, 宁夏 银川 750004
  • 2. 宁夏回族自治区疾病预防控制中心, 宁夏 银川 750003
  • 3. 宁夏医科大学公共卫生与管理学院, 宁夏 银川 750004;宁夏医科大学基础医学院, 宁夏 银川 750004
  • 折叠

摘要

目的 建立GC-MS法同时测定枸杞中 16 种农药残留量的含量,并进行安全性评价.方法 分析采用DB-5MS色谱柱(30 m×0.25 mm,0.25 μm);程序升温;进样量 1.0 μL,不分流;体积流量 1.0 mL/min;进样口温度 250℃;电子轰击电离(EI),电子能量 70 eV;离子源温度 230℃;多反应监测模式;碰撞气高纯N2.采用残留水平、膳食摄入风险、风险排序和累积暴露评估对农药残留膳食风险相对较高的农药进行分析与讨论.结果 16 种农药在各自范围内线性关系良好(r≥0.994 4),平均加样回收率 70%~114%,RSD小于2%.产地枸杞和商超枸杞均未出现农药残留超标情况;产地枸杞中氟氯氰菊酯的平均残留量最高,为 0.999 2 mg/kg,商超枸杞中氯氰菊酯的平均残留量最高,为 0.088 4 mg/kg;产地枸杞和商超枸杞的慢性和急性膳食风险最高的农药均是氯氰菊酯;溴氰菊酯、哒螨灵、毒死蜱、敌敌畏、杀扑磷风险较高,但实际检测中只有哒螨灵被检出,并且未超标;产地、商超枸杞慢性危害指数(HI)值分别为 0.012 9、0.001 2,急性HI值分别为0.065 5、0.005 4.结论 部分枸杞样品存在农药残留,但均处于安全水平,喷洒农药时需要注意氯氰菊酯的使用.

Abstract

AIM To establish a GC-MS method for the simultaneous content determination of sixteen pesticide residues in Lycii Fructus and perform safety assessment.METHODS The analysis was performed on DB-5MS chromatographic column(30 m×0.25 mm,0.25 μm)subjected to the programmed heating,with splitless injection of 1.0 μL dissolved sample at a flowing rate of 1.0 mL/min.Other parameters were as follows:injection port temperature of 250℃,electron impact ionization(EI),electron energy of 70 eV;ion source temperature of 230℃,multi-reaction monitoring mode,and collision gas.of high-purity N2.Pesticide residues with relatively high dietary risk were analyzed and discussed with regard to residue levels,dietary intake risk,risk ranking and cumulative exposure assessment.RESULTS Sixteen pesticides showed good linear relationships within their own ranges(r≥0.994 4),whose average recoveries were 70%-114%,with the RSDs of less than 2%.The highest average cyfluthrin residue of 0.999 2 mg/kg in Lycii Fructus of production regions and the highest average cypermethrin residue of 0.088 4 mg/kg in Lycii Fructus commodities were both detected.In Lycii Fructus of production regions with chronic hazard index(HI)value of 0.012 9 and acute HI value of 0.065 5 and their commodities with chronic HI of 0.001 2 and acute HI of 0.005 4,the pesticide residue of cypermethrin was the leading cause of chronic and acute dietary risk,and additionally,pyridaben within maximum residue limit(MRL)was the only detectectable highly toxic pesticide among the other most concerning pestcides of deltamethrin,pyridaben,chlorpyrifos,dichlorvos and methidathion.CONCLUSION There exist pesticide residues within MRL values in some samples of Lycii Fructus and the use of cypermethrin should be well-controlled.

关键词

枸杞/农药残留/GC-MS/风险评估

Key words

Lycii Fructus/pesticide residues/GC-MS/risk assessment

引用本文复制引用

基金项目

国家自然科学基金资助项目(21667023)

国家自然科学基金资助项目(21966025)

教育部春晖计划资助项目(Z2016068)

出版年

2024
中成药
国家食品药品监督管理局,信息中心中成药信息站,上海中药行业协会

中成药

CSTPCDCSCD北大核心
影响因子:1.217
ISSN:1001-1528
参考文献量16
段落导航相关论文