超高效液相色谱-串联质谱法测定烟草中抑芽丹残留

Determination of maleic hydrazide residues in tobacco by using ultra performance liquid chromatography-tandem mass spectrometry

建立一种新型样品萃取瓶结合超高效液相色谱-串联质谱(UPLC-MS/MS)测定烟草中抑芽丹的方法。经萃取过滤后的样品用UPLC-MS/MS测定,以20%的乙腈为流动相,流速0.5 mL/min,采用ACQUITY UPLC BEH HILIC(2.1 mm×50 mm,1.7μm)为色谱分离柱。采用新型的样品萃取瓶可以集样品萃取、过滤和转移为一体,大大简化了前处理步骤;抑芽丹在0.05~5.0μg/mL范围内具有较好的线性,线性相关系数>0.999;方法检测限为0.25 mg/kg;在不同添加水平下,回收率为94.60%~110.08%,相对标准偏差(RSD)<5%(n=5),具有较好的重复性。此方法能较好的应用于烟草中抑芽丹残留量的测定。

To establish a new extraction vial device coupled with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the determination of maleic hydrazide residues.The prepared sample was tested by UPLC-MS/MS.The separation was performed on ACQUITY UPLC BEH HILIC column(2.1 mm×50 mm,1.7μm),taking 20%acetonitrile as the mobile phase at a flow-rate of 0.5 mL/min.It’s shown that the novel extraction vial was simple,easy operation and coupling extraction,filtering with transfer for one step.The calibration curves showed a good linearity in the range of 0.05~0.5μg/mL with the correlation coefficients larger than 0.999.The limits of detection(LOD)was confirmed at 0.25 mg/g.The extraction recoveries range from 94.60%~110.08%in different spiked concentrations samples and the relative standard deviation was less than 5%(n=5).The detection method was suitable for the monitoring analysis for maleic hydrazide residues in tobacco.