液相色谱-串联质谱法检测水稻中噁唑酰草胺及其代谢物残留

Determination of Metamifop and Its Metabolites in Rice by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry

建立了超高效液相色谱-串联质谱(UPLC-MS/MS)快速检测水稻植株、稻壳、糙米中噁唑酰草胺及其代谢物(HFMPA、HPFMPA、6-CBO)残留量的方法。样品用乙腈提取PSA净化处理,过0.22μm有机系滤膜后,以乙腈-甲酸水为流动相,在电喷雾正离子模式下以多反应监测(MRM)模式测定,用标准溶液外标法定量。结果表明:方法的线性范围为0.05~1.00 mg·kg^-1,决定系数(R^2)>0.99;在0.05、0.50、1.00 mg·kg^-13个添加水平下,该方法平均回收率为82%~109%,相对标准偏差为2%~8%,定量限为0.01 mg·kg^-1。该处理方法操作简便快速、准确率高、灵敏度高,适用于实际操作,是水稻中噁唑酰草胺及其代谢物(HFMPA、HPFMPA、6-CBO)残留检测较理想的办法。

A method for the rapid determination of oxazolylamine and its metabolites(hfmpa,hpfmpa,6-cbo)residues in rice plants,husks and brown rice by ultra high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)was established.Samples were extracted with acetonitrile and purified by PSA.After 0.22 m organic filtration membrane,acetonitrile/formic acid water was used as mobile phase.In the electrospray ionization mode,the multi reaction monitoring(MRM)mode was used to measure the samples.The results showed that the linear range of the method was 0.05~1.00 mg·kg^-1,and the determination coefficient(R^2)was more than 0.99.At the three levels of 0.05,0.50 and 1.00 mg·kg^-1,the average recovery of the method was 82%~109%,the relative standard deviation was 2%~8%,and the quantitative limit was 0.01 mg·kg^-1.This method is simple,rapid,accurate and sensitive.It is suitable for practical operation.It is an ideal method for the detection of oxazolylamine and its metabolites(hfmpa,hpfmpa,6-cbo)residues in rice.