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

作　　者：王康 陈慧 肖少红 李韵 

机构地区：[1]湖北省烟草产品质量监督检验站,武汉市硚口区宝丰路6号430030

出　　处：《烟草科技》2018年第2期48-54,共7页Tobacco Science & Technology

基　　金：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)

摘　　要：为准确测定烟草及烟草制品中抑芽丹的残留量,建立了一种固相萃取-超高效液相色谱-串联质谱(SPE-UPLC-MS/MS)方法。烟草样品经盐酸溶液加热回流提取、石墨化炭黑(GCB)SPE柱净化后在多反应监测负离子模式下测定,采用氘代抑芽丹同位素内标法定量。结果表明:(1)使用石墨化炭黑SPE柱可有效净化萃取液,除去盐酸后的洗脱液pH近中性,适合于质谱分析;(2)抑芽丹定量限为0.47 mg/kg,回收率为94.2%~102.1%,相对标准偏差(RSD)小于6%;(3)采用该方法检测了13个烟草样品中的抑芽丹残留量,并与采用YC/T 405.5—2011标准方法的测定值进行比较,结果显示两组数据的一致性较好。该方法灵敏度高,稳定性和准确性好,适用于烟草样品中抑芽丹残留量的测定。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 

分 类 号：S481.8[农业科学—农药学]