烟草科技2018，Vol.51Issue(2)：48-54,7.
SPE-UPLC-MS/MS法测定烟草及烟草制品中抑芽丹残留量
Determination of maleic hydrazide residues in tobacco and tobacco products by SPE-UPLC-MS/MS
摘要
Abstract
To determine the maleic hydrazide residues in tobacco and tobacco products, an SPE-UPLC-MS/MS method was developed by adopting solid phase extraction cartridges (SPE) for sample clean-up and ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) for detection. Tobacco samples were extracted with hydrochloric acid under heating and refluxing, and further purified by solid-phase clean-up with graphitized carbon black (GCB) column. The ESI source in negative ion mode was used for qualitative and quantitative analyses under multiple reaction monitoring (MRM) mode with d2-maleic hydrazide as the internal standard. The results showed that: 1) After the purification by GCB column, the pH value of the eluent was near neutral after removing hydrochloric acid. 2) The limit of quantification was 0.47 mg/kg, and recoveries ranged from 94.2% to 102.1% with relative standard deviation (RSD) less than 6%. 3) The maleic hydrazide residues in 13 tobacco samples were detected by this method and compared with those determined by the standard method described in YC/T 405.5-2011, the data using the two methods agreed with each other very well. This method is sensitive, stable, accurate and suitable for determining the maleic hydrazide residues in tobacco samples.关键词
石墨化炭黑SPE柱/抑芽丹/烟草/烟草制品/负离子模式Key words
GCB column/Maleic hydrazide/Tobacco/Tobacco product/Negative ion mode分类
农业科技引用本文复制引用
王康,陈慧,肖少红,李韵..SPE-UPLC-MS/MS法测定烟草及烟草制品中抑芽丹残留量[J].烟草科技,2018,51(2):48-54,7.基金项目
国家烟草专卖局烟草行业标准制修订项目"烟草及烟草制品抑芽丹农药残留量的测定液相色谱-串联质谱法"(562017AB0050). （562017AB0050）
