QuEChERS-气相色谱-串联质谱法测定黄瓜中10种农药残留

Determination of ten pesticide residues in cucumber using QuEChERSgas chromatography-tandem mass spectrometry

建立了黄瓜中氟啶虫酰胺、丁苯吗啉、氟吡菌酰胺、氟啶虫胺腈、环酰菌胺、氟吡菌胺、唑嘧菌胺、氟吗啉、烯肟菌酯和烯肟菌胺10种农药残留的QuEChERS-气相色谱-串联质谱检测方法。样品采用QuEChERS方法,经乙腈涡旋振荡提取,无水硫酸镁和氯化钠盐析后,取5 mL提取液,加入含125 mg PSA、900 mg无水MgSO_4和25 mg GCB的组合净化剂进行净化,采用Agilent HP-5 MS Ultra Inert色谱柱分离,气相色谱-串联质谱仪多反应监测(MRM)模式测定,基质匹配标准曲线外标法定量。结果表明:在检测浓度范围内,10种农药的质量浓度与其对应的峰面积间呈良好线性关系,决定系数均大于0.99;10种农药的平均回收率在76%～105%之间,相对标准偏差在4.0%～12%之间,定量限在0.001～0.05 mg/kg之间。该方法简便、快速、可靠,适用于黄瓜中10种农药残留的快速检测和分析确证。

A multiresidue analytical method for the determination of 10 pesticide(flonicamid、fenpropimorph、fluopyram、sulfoxaflor、fenhexamid、fluopicolide、ametoctradin、flumorph、enestroburin and fenaminstrobin) residues in cucumber was developed using QuEChERS-gas chromatography-tandem mass spectrometry(GC-MS/MS).The target compound were extracted with acetonitrile by QuEChERS method. After salting out of anhydrous magnesium sulfate(MgSO4) and sodium chloride(NaCl), 5 mL extraction solvent was cleaned up and purified by a mixed sorbent of 125 mg PSA, 900 mg MgSO4 and 25 mg GCB. The samples was then separated on an Agilent HP-5 MS Ultra Inert column and wsa detected by GC-MS/MS system with the external standard method using matrix matched calibration curves. Results showed that linear relationships between peak area and mass concentration of 10 pesticides were achieved with a determination coefficient of 0.99. The recoveries ranged from 76% to 105% at four spiked levels in cucumber and the relative standard deviations(RSDs) ranged from 4.0% to 12%. The limits of quantification(LOQs) of the method were from 0.001mg/kg to 0.05 mg/kg. This new method is suitable for the rapid and accurate determination of the 10 pesticide residues in cucumber.