硫酸铜处理-气相色谱法测定洋葱中12种有机磷农药残留  

Determination of 12 kinds of organophosphorus pesticide residues in onion by copper sulfate treatment-gas chromatography

作　　者：熊俊杰 刘超 尹海飞 柴连周[2] 张绍龙 黄娜 李云刚 张多丽 何家转 XIONG Jun-Jie;LIU Chao;YIN Hai-Fei;CHAI Lian-Zhou;ZHANG Shao-Long;HUANG Na;LI Yun-Gang;ZHANG Duo-Li;HE Jia-Zhuan(Baoshan Qualityand Technical Supervision Comprehensive Testing Center,Baoshan 678000,China;Baoshan College of Tradiitonal Chinese Medicine,Baoshan 678000,China)

机构地区：[1]保山市质量技术监督综合检测中心,保山678000 [2]保山中医药高等专科学校,保山678000

出　　处：《食品安全质量检测学报》2021年第6期2246-2251,共6页Journal of Food Safety and Quality

基　　金：保山中医药高等专科学校百名中青年学术带头人资助项目(2020×002)。

摘　　要：目的建立硫酸铜处理-气相色谱法同时测定洋葱中12种有机磷类农药残留的分析方法。方法样品在破碎前加入5%硫酸铜溶液,用乙腈超声提取,TPC固相萃取柱净化,浓缩后供气相色谱检测。结果5%硫酸铜溶液较好地去除了洋葱中硫化物的干扰,12种有机磷农药在给定的条件下得到良好分离,在0.02~0.2μg/mL浓度范围内,方法线性良好,相关系数r均大于0.99,12种有机磷类农药在0.05、0.1和0.5mg/kg添加水平的回收率为70.0%~109.8%,相对标准偏差在3.0%~17.8%之间,检出限在0.010~0.015 mg/kg之间,定量限在0.033~0.050 mg/kg。结论采用硫酸铜前处理能显著减少洋葱样品中硫化物对有机磷类农药残留检测的干扰,该方法简便、快捷、准确,为洋葱的检测提供了一种有效的方法。Objective To establish a method for the simultaneous determination of 12 kinds of organophosphorus pesticide residues in onion by copper sulfate treatment and gas chromatography.Methods The 5%copper sulfate solution was added to the sample before crushing,ultrasonic extraction with acetonitrile,purification with TPC solid phase extraction column,and it was detected by gas chromatography after concentration.Results The 5%CuSO4 solution could remove the interference of sulfide in onion,and 12 kinds of organophosphorus pesticides were well separated under the given conditions.The linear range was 0.02-0.2μg/mL,and the correlation coefficient r was more than 0.99.The recoveries of 12 kinds of organophosphorus pesticides at the levels of 0.05,0.1 and 0.5 mg/kg were 70.0%-109.8%,and the relative standard deviations were 3.0%-17.8%.The detection limit was 0.010-0.015 mg/kg and the quantitation limit was 0.033-0.050 mg/kg.Conclusion Copper sulfate pretreatment can significantly reduce the interference of sulfide in onion samples on the detection of organophosphorus pesticide residues.This method is simple,rapid and accurate,which provides an effective method for the detection of onion.

关 键 词：硫酸铜 气相色谱法 洋葱 有机磷农药 

分 类 号：O657.71[理学—分析化学] TS255.7[理学—化学]