GC-MS/MS法测定大米、砀山梨及娃娃菜中胺鲜酯的残留量

Determination of Residual Diethyl Aminoethyl Hexanoate in Rice,Dangshan Pear and Baby Cabbage by GC-MS/MS Method

建立了一种适用于气相色谱-串联质谱联用仪测定蔬菜、水果、粮谷中胺鲜酯残留量的分析方法。试样经过乙腈提取,QuEChERS dSPE EMR-Lipid(大米试样)、PSA、C_(18)及GCB(砀山梨和娃娃菜试样)净化后,以HP-5MS色谱柱进行分离,在电子轰击离子源、多反应监测模式下检测大米、砀山梨和娃娃菜中胺鲜酯的残留量,基质外标法定量。结果表明,胺鲜酯浓度在2~200 ng·mL^(-1)时,线性关系良好,相关系数(r)均在0.9999以上,在3个不同浓度添加水平下,大米胺鲜酯的回收率为92.4%~105.0%,砀山梨胺鲜酯的回收率为84.0%~90.0%,娃娃菜胺鲜酯的回收率为93.6%~112.0%,大米的方法检出限为0.002 mg·kg^(-1),定量限为0.004 mg·kg^(-1);砀山梨和娃娃菜的检出限为0.001 mg·kg^(-1),定量限为0.002 mg·kg^(-1)。方法精密度试验的相对标准偏差在5%以内。该方法适用于蔬菜、水果、粮谷中胺鲜酯的定性和定量测定。

A gas chromatography-tandem mass spectrometry method was developed for the determination of residual diethyl aminoethyl hexanoate in vegetables,fruits and grains.The sample is extracted by acetonitrile,purified by QuEChERS dSPE EMR-Lipid(rice sample),purified by PSA,C_(18),and GCB(Dangshan pear and baby cabbage sample),and separated by HP-5MS column.The residues of diethyl aminoethyl hexanoate in rice,Dangshan pear and baby cabbage were detected by electron bombardment ion source and multi-party monitoring mode.Quantification by matrix external standard method.The results show that the concentration of DA-6 is in the range of 2~200 ng·mL^(-1).The linear relationship was good,and the correlation coefficients(r)were all above 0.9999.At three different concentration addition levels,the recovery rate of rice DA-6 were 92.4%~105.0%,the recovery rate of Dangshan pear DA-6 were 84.0%~90.0%,the recovery rate of baby cabbage DA-6 is 93.6%~112.0%.The detection limit for rice is 0.002 mg·kg^(-1),and the quantification limit is 0.004 mg·kg^(-1);the detection limit for Dangshan pear and baby cabbage is 0.001 mg·kg^(-1),and the quantitative limit is 0.002 mg·kg^(-1).The relative standard deviation of the method precision test is within 5%.This method is suitable for the qualitative and quantitative determination of diethyl aminoethyl hexanoate in vegetables,fruits,and grains.