摘要
建立了韭菜中19种农药残留的气相色谱-质谱(GC-MS)分析方法。样品前处理采用QuEChERS方法,用乙腈溶液进行提取,经N-丙基乙二胺(PSA)、十八烷基硅烷键合硅胶(C18)、石墨化炭黑(GCB)和无水硫酸镁固相分散净化,浓缩定容后用GC-MS在选择离子监测模式(SIM)下进行测定,外标法定量。结果显示,19种农药在线性范围内相关系数均大于0.99。方法检出限为0.001~0.041 mg/kg,方法定量限为0.004~0.136 mg/kg,添加水平分别为0.2,0.4和1.0 mg/kg,回收率为82.0%~109.9%,相对标准偏差为0.7%~2.8%(n=6)。该方法前处理过程简单、快速,灵敏度高,重现性好,适用于韭菜中19种农药残留的测定。
A rapid method was developed for the simultaneous determination of 19 pesticide residues in Chinese chives by gas chromatography-mass spectrometry.The samples were prepared by the modified QuEChERS method,extracted with acetonitrile,and cleaned-up by adding primary secondary amine(PSA),octadecyl silane chemically bonded silica(C18),graphitized carbon black(GCB)and anhydrous magnesium sulfate.After concentration and dissolution,the 19 target compounds were analyzed by GC-MS under selected ion monitoring(SIM)mode.The external standard method was used for quantitative analysis.The results showed that all the linear relationships were good with the correlation coefficients all greater than 0.99.The limits of detection of the method were 0.001-0.041 mg/kg,the limits of quantitation were 0.004-0.136 mg/kg,and the recoveries ranged from 82.0%-109.9%in spiked level of 0.2,0.4 and 1.0 mg/kg,with the relative standard deviations of 0.7%-2.8%(n=6).The method was simple,accurate,sensitive and suitable for the determination of 19 pesticide residues in Chinese chives.
作者
马楠
张玉娟
张志强
MA Nan;ZHANG Yujuan;ZHANG Zhiqiang(Xingtai Customs of People’s Republic of China,Xingtai 054000)
出处
《食品工业》
CAS
北大核心
2020年第1期323-326,共4页
The Food Industry
