食品科学 ›› 2023, Vol. 44 ›› Issue (20): 387-392.doi: 10.7506/spkx1002-6630-20220928-311

• 安全检测 • 上一篇    

碳气凝胶分散固相萃取-气相色谱法检测蔬果中有机磷农药残留

操江飞,谢春生,李志安,黄象金,韦寿莲   

  1. (1.肇庆学院环境与化学工程学院,广东 肇庆 526061;2.广东省环境健康与资源利用重点实验室,广东 肇庆 526061;3.肇庆市食品检验所,广东 肇庆 526060)
  • 出版日期:2023-10-25 发布日期:2023-11-07
  • 基金资助:
    2021年肇庆市省乡村振兴战略专项(2021N001);广东省省级大学生创新训练项目(S202210580066); 广东省环境健康与资源利用重点实验室项目(2020B121201014)

Determination of Organophosphorus Pesticide Residues in Vegetables by Carbon Aerogel Dispersive Solid Phase Extraction Combined with Gas Chromatography

CAO Jiangfei, XIE Chunsheng, LI Zhi’an, HUANG Xiangjin, WEI Shoulian   

  1. (1. School of Environmental and Chemical Engineering, Zhaoqing University, Zhaoqing 526061, China; 2. Guangdong Provincial Key Laboratory of Environmental Health and Land Resource, Zhaoqing 526061, China; 3. Zhaoqing Institute for Food Control, Zhaoqing 526060, China)
  • Online:2023-10-25 Published:2023-11-07

摘要: 建立碳气凝胶分散固相萃取-气相色谱法测定蔬菜水果中治螟磷、乐果、杀螟硫磷、对硫磷、杀扑磷、三唑磷、益棉磷农药残留的方法,优化提取剂种类、提取时间、氯化钠用量、净化剂用量、净化时间。结果表明,以乙腈为提取剂,碳气凝胶用量15 mg、氯化钠2.0 g、提取6 min、净化时间0.5 min条件下,7 种有机磷类农药在0.01~3.0 µg/mL范围内具有良好的线性关系,相关系数为0.999 0~0.999 8,检出限(RSN=3)为0.4~1.0 μg/kg,样品加标3 个水平实验的回收率均在85.5%~102%之间。本方法操作简便、快速,材料制作成本低,适用于果蔬样品中检测有机磷农药残留量。

关键词: 蔬菜水果;气相色谱法;碳气凝胶;有机磷农药;分散固相萃取

Abstract: A method for the determination of sulfotep, dimethoate, fenitrothion, parathion, methidathion, triazophos and azinos residues in vegetables and fruits by dispersive solid phase extraction (SPE) using a carbon aerogel-based sorbent combined with gas chromatography (GC) was developed. Solvent type, extraction time, the amounts of sodium chloride and purifying agent, and purification time were optimized. The results showed that the optimum conditions were determined as follows: acetonitrile as extraction solvent, 15 mg of carbon aerogel, 2.0 g of sodium chloride, extraction time 6 min, and purification time of 0.5 min. Under these conditions, good linearity was observed for all analytes in the concentration range of 0.01–3.0 μg/mL, with correlation coefficients of 0.999 0–0.999 8, and the detection limit at a signal to noise ratio of 3 was 0.4–1.0 μg/kg. The mean recoveries of spiked samples at three concentrations were 85.5%–102%. The developed method is simple, rapid, low-cost and suitable for the determination of organophosphorus pesticide residues in fruit and vegetable samples.

Key words: vegetables and fruits; gas chromatography; carbon aerogel; organophosphorus pesticides; dispersive solid phase extraction

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