QuEChERS-液相色谱-串联质谱法测定生咖啡中19种琥珀酸脱氢酶抑制剂类杀菌剂残留

Determination of 19 Succinate Dehydrogenase Inhibitor Fungicides Pesticide Residues in Green Coffee by Quechers-Liquid Chromatography Tandem Mass Spectrometry

本研究旨在建立QuEChERS前处理技术结合液相色谱串联质谱仪(LC-MS/MS)同时测定生咖啡中19种琥珀酸脱氢酶抑制剂(Succinate dehydrogenase inhibitor)杀菌剂残留量的分析方法。生咖啡粉末样品经乙腈均值提取,采用无水硫酸镁、PSA、C18净化剂净化,经液相色谱–串联质谱仪在正离子模式下扫描分析19种琥珀酸脱氢酶抑制剂类杀菌剂残留,通过空白基质匹配标准溶液外标法定量。19种琥珀酸脱氢酶抑制剂类杀菌剂在1~100 ng/mL范围内呈良好线性关系(r>0.995),在0.01、0.05和0.1 mg/kg的加标水平下,平均回收率为79.6%~109.4%,相对标准偏差(relative standard deviations,RSD,n=6)为1.4%~9.7%,方法检出限为0.51~4.60μg/kg。该方法具有良好的线性关系,准确度和精密度均满足定量分析的要求,适用于生咖啡中19种琥珀酸脱氢酶抑制剂类杀菌剂农药残留的定量分析。

This study establishes an analytical method for simultaneous determination of 19 Succinate dehydrogenase inhibitor fungicides pesticide residues in Green coffee by QuEChERS-Liquid chromatography tandem mass spectrometry.The Green coffee powder samples were extracted with acetonitrile by Homogenizer,the supernatant were purified by Magnesium sulfate anhydrous、PSA and C18,liquid chromatograhy-tandem mass spectrometry were used for analyzing 19 Succinate dehydrogenase inhibitor fungicides pesticide residues at positive ion mode.The results showed that the calibration curves of 19 targets showed good linearity with correlation coefficients of above 0.9950 in the range of 1~100 ng/mL,the recoveries of 19 pesticides were 79.6%~109.4%and the relative standard deviations(RSD,n=6)were in the range of 1.4%~9.7%at spiked levels of 0.01、0.05 and 0.1 mg/kg.Limit of quantitation(LOQ)of all the tested pesticides were 0.51~4.60μg/kg.This method has good linear relations,excellent stable and sensitive,accuracy and precision meet the requirement of quantitative analysis,it is suitable for quantitative analysis of 19 Succinate dehydrogenase inhibitor fungicides pesticide residues in Green coffee.