气相色谱-三重四极杆串联质谱法测定蔓越橘提取物中的88种农药残留

Determination of 88 pesticide residues in cranberry plant extract by gas chromatography-triple quadrupole tandem mass spectrometry

采用改进的快速、简单、便宜、有效、稳定和可靠的前处理方法(quick,easy,cheap,effective,rugged,safe,即QuEChERS法),结合气相色谱-三重四极杆串联质谱(GC-MS/MS)检测技术,建立了蔓越橘提取物中88种农药残留的分析方法。样品由含1%乙酸的丙酮-正己烷(1∶1,v/v)溶剂提取,乙二胺-N-丙基甲硅烷(PSA)与石墨化碳(GCB)净化后,采用GC-MS/MS技术在多反应监测(MRM)模式下测定,外标法定量。蔓越橘提取物中88种农药在0.001～0.2 mg/L范围内线性关系均良好;所有农药的方法定量限(LOQ,信噪比(S/N)≥10)均低于31.5μg/kg;在5、25和50μg/kg添加水平下,88种农药的平均回收率为71.4%～116.6%,相对标准偏差(RSD)为2.4%～16.9%。该方法样品前处理简单快速,灵敏度、准确度和精密度均符合农药多残留检测技术的要求,适用于蔓越橘提取物中88种农药残留的快速筛查测定。

A method by using a modified QuEChERS（quick,easy,cheap,effective,rugged and safe） and gas chromatography-triple quadrupole tandem mass spectrometry（GC-MS/MS） was established to analyze 88 pesticide residues in cranberry plant extract.The sample was extracted with acetone-hexane（1∶1,v/v） containing 1% acetic acid,then cleaned-up by ethylenediamine-N-propyl silyl（PSA） and graphite carbon（GCB）.The extract was determined by GC-MS/MS in multi-reaction monitoring（MRM） mode,and external standard method was applied to quantified the pesticides.All the 88 pesticides showed good linearity in the range of 0.001-0.2 mg/L,and the limits of quantification（LOQs,S/N≥10） were all less than 31.5 μg/kg.The average recoveries of all the pesticides were in the range of 71.4% to 116.6% at three spiked levels of 5,25 and 50 μg/kg in cranberry plant extract,with the relative standard deviations（RSDs） of 2.4%-16.9%.The results demonstrated that this method is simple,rapid and suitable for the determination of 88 pesticide residues in cranberry plant extract.The analytical sensitivity and accuracy can meet the requirements of multiple pesticide residue analysis.