QuEChERS-气相色谱-串联质谱法测定果蔬中乙烯菌核利及其代谢物的残留量

QuEChERS-Gas Chromatography Tandem Mass Spectrometry for the Determination of Vinclozolin and Its Metabolite Residues in Fruits and Vegetables

建立了改进的QuEChERS方法结合气相色谱/质谱(GC/MS)法快速测定果蔬中乙烯菌核利及其代谢物3,5-二氯苯胺残留量的方法。研究改良了QuEChERS方法中吸附剂的种类和用量,用乙酸乙酯提取番茄、黄瓜、生菜、芹菜、柑橘和葡萄中乙烯菌核利及其代谢物残留,经乙二胺-N-丙基硅烷(PSA)粉80 mg、石墨化碳黑(GCB)粉50 mg吸附杂质净化后,GC/MS外标法定量。结果表明,乙烯菌核利及其代谢物3,5-二氯苯胺在0.02~0.25μg/mL的质量浓度范围内呈线性关系,相关系数为0.997和0.998。乙烯菌核利及其代谢物在番茄、黄瓜、生菜、芹菜、柑橘和葡萄中的添加水平为0.05~3.0 mg/kg时平均回收率范围均处于81.67%~113.33%之间,相对标准偏差(RSD)小于9.47%,方法的检出限(LOD,S/N=3)乙烯菌核利在4.2~15.5μg/kg之间,3,5-二氯苯胺在6.3~17.6μg/kg之间。本方法具有快速、简便、灵敏等特点,能满足果蔬中残留乙烯菌核利及其代谢物的检测要求。

An improved QuEChERS method combined with gas chromatography/mass spectrometry(GC/MS)method was established for the rapid determination of vinclozolin and its metabolite,3,5-dichloroaniline residue,in fruits and vegetables.This research improved the type and amount of adsorbent in QuEChERS method.Vinclozolin and its metabolite residues in tomatoes,cucumbers,lettuce,celery,citrus and grapes were extracted with ethyl acetate.The extract was purified using 80 mg of PSA and 50 mg of GCB to remove impurities via adsorption,before quantification by GC/MS with external standards.The results showed that vinclozolin and its metabolite 3,5-dichloroaniline showed a linear relationship in the mass concentration range of 0.02~0.25 mg/mL,with the correlation coefficients as 0.997 and 0.998 respectively.The average recovery range of vinclozolin and its metabolite in tomatoes,cucumbers,lettuce,celery,citrus and grapes was between 81.67%and 113.33%at the spiked level of 0.05~3.0 mg/kg,with the relative standard deviations(RSDs)less than 9.47%.The limits of detection(LOD,S/N=3)were between 4.2 and 15.5μg/kg for vinclozolin,and between 6.3 and 17.6μg/kg for 3,5-dichloroaniline.This method is rapid,simple and sensitive,and can meet the detection requirements of residual vinclozolin and its metabolites in fruits and vegetables.