提出了高效液相色谱-串联质谱法测定生姜中涕灭威及其代谢物涕灭威亚砜、涕灭威砜的残留量。样品经乙腈均质提取,氨基固相萃取柱净化后,用YMC C18色谱柱分离,采用电喷雾离子化正离子模式及多反应监测模式进行测定。涕灭威、涕灭威亚砜和涕灭威砜的测定下限(10S/N)均为1 μg·kg-1。在3个标准加入水平下进行了回收率和精密度试验,方法的回收率在64.1%~114%之间,测定值的相对标准偏差(n=6)在1.5%~4.9%之间。

A method of HPLC-MS/MS for the determination of residual amounts of aldicarb and its metabolites, including aldicarb-sulfoxide and aldicarb-sulfone in ginger was proposed. Samples were extracted with acetonitrile, and the extract was concentrated and purified on NH2-solid phase extraction tube. The YMC C18 column was used as chromatographic column, and positive electrospray ionization as well as multiple reactions monitoring mode were used in the detection. Values of lower limit of determination (10S/N) of aldicarb, aldicarb-sulfoxide and aldicarb-sulfone found were 1 μg·kg-1. Tests for recovery and precision were made by addition of standard solution of the 3 compounds at 3 different concentration levels to ginger samples which were analyzed by the proposed method. Values of recovery found were in the range of 64.1%-114%, and values of RSD′s (n=6) found were in the range of 1.5%-4.9%.