枸杞中乙基多杀菌素及其代谢物的检测方法

Detection Method of Spinetoram and Its Metabolites in Lycium Fruit

[目的]利用超高效液相色谱串联质谱法,对枸杞鲜干果实中乙基多杀菌素L(XDE-175-L)、乙基多杀菌素J(XDE-175-J)及其代谢物N-demethyl-XDE-175-J、N-formyl-XDE-175-J进行检测。[方法]枸杞样品用乙腈提取,N-丙基乙二胺(PSA)和石墨化炭(GCB)净化后,采用超高效液相色谱-三重四级杆质谱联用仪检测,外标法定量。[结果]乙基多杀菌素及其代谢物在枸杞鲜果中平均回收率为80.3%~188.7%,相对标准偏差为0.3%~19.1%,在枸杞干果中平均回收率为84.8%~112.8%,相对标准偏差为2.2%~19.3%,定量限为0.01 mg/kg。[结论]该方法可以准确、快速测定枸杞中乙基多杀菌素及其代谢物。

[Aims]Spinetoram L(XDE-175-L),XDE-175-J and its metabolites N-demethyl-XDE-175-J,N-formyl-XDE-175-J residues in Lycium fruit were detected by liquid chromatography mass spectrometer(LC-MS/MS).[Methods]Lycium fruit samples were extracted with acetonitrile,purified with 50 mg PSA and 10 mg GCB,then detected and quantified by external standard method.[Results]The results showed that the recovery rate of spinetoram and its metabolites in fresh fruit was 80.3-188.7%,the relative standard deviation was 0.3-19.1%,and the recovery rate in dried fruit was 84.8-112.8%.The deviation was 2.2-19.3%,and the limit of quantification was 0.01 mg/kg.[Conclusions]This method can accurately and quickly determine the spinosyn and its metabolites.