摘要
目的建立微波辅助净化-气相色谱法测定含硫蔬菜中有机磷农药残留的分析方法。方法样品经微波预处理抑制酶促反应后,使用乙腈提取、基质分散固相萃取净化、丙酮复溶、有机滤膜过滤后,采用气相色谱-火焰光度检测器测定。结果敌敌畏、甲胺磷、氧乐果、乐果、毒死蜱、水胺硫磷在0.01~0.50μg/mL浓度范围内呈现良好的线性关系,相关系数均大于0.999,方法的检出限为0.0002~0.0004 mg/kg,定量限为0.0008~0.0013 mg/kg;有机磷农药在香葱、韭菜、白萝卜基质中加标0.002,0.010,0.100 mg/kg浓度水平,加标回收率为83.2%~104.7%,相对标准偏差在2.3%~10.2%(n=6)。结论本方法简便,抗干扰能力强,定量准确,具有良好的重现性和稳定性,能够有效的检测含硫蔬菜中有机磷农残的含量。
Objective To establish a method for determination of organophosphorus pesticide residues in sulfur-containing vegetables by gas chromatography with microwave-assisted clean-up treatment.Methods After microwave pretreatment of the sample to inhibit the enzymatic reaction,the sample was extracted with acetonitrile,purified by matrix-dispersed solid phase extraction,reconstituted with acetone,and filtered with an organic filter,and then determined by gas chromatography-flame photodetector.Results Dichlorvos,methamidophos,omethoate,dimethoate,chlorpyrifos,and amithion exhibited good linear relationship in the concentration range of 0.01-0.50μg/mL,the correlation coefficients were all greater than 0.999 mg/kg,and the limits of quantitation were 0.0008-0.0013 mg/kg.Organophosphorus pesticides spiked in chives,leeks,and white radish matrices at 0.002,0.010,0.100 mg/kg,the spiked recovery was 83.2%-104.7%,and the relative standard deviation was 2.3%-10.2%(n=6).Conclusion This method is simple,and has strong anti-interference ability,accurate quantification,good reproducibility and stability,which can effectively detect the content of organophosphorus pesticide residues in sulfur-containing vegetables.
作者
巫立健
WU Li-Jian(Center for Food and Drug Inspection and Testing of Nanping,Nanping 353000,China)
出处
《食品安全质量检测学报》
CAS
2020年第2期607-613,共7页
Journal of Food Safety and Quality
关键词
有机磷农药残留
微波辅助净化
基质分散固相萃取
含硫蔬菜
气相色谱法
organophosphorus pesticide residues
microwave-assisted clean-up treatment
matrix dispersive solid phase extraction
sulfur-containing vegetables
gas chromatography
