采用高效液相色谱-双柱后反应-荧光检测法测定烟草中的涕灭威、涕灭威亚砜和涕灭威砜。

Determination of aldicarb, aldicarb sulfoxide and aldicarb sulfone in tobacco using high-performance liquid chromatography with dual post-column reaction and fluorescence detection.

作者信息

Yang S S, Smetena I

机构信息

Research Center, Philip Morris USA, Richmond, VA 23261.

出版信息

J Chromatogr A. 1994 Apr 1;664(2):289-94. doi: 10.1016/0021-9673(94)87019-5.

DOI:10.1016/0021-9673(94)87019-5

PMID:8199709

Abstract

A screening method for the determination of aldicarb (AS) and its sulfoxide (ASX) and sulfone (ASN) metabolites in tobacco at low ppm levels is described. Tobacco samples are extracted using methanol with the aid of sonication at ambient conditions. The extract is filtered and then injected into a high-performance liquid chromatograph equipped with a dual post-column reaction system and a fluorescence detector. Chromatographic separation is performed on a C18 column with a mixture of methanol-acetonitrile-water containing 0.1% of triethanolamine as the mobile phase. Triethanolamine is added to improve peak shape of AS residues and to reduce the undesired interaction between residual silanols and interferences, mainly amino acids and other amines. The average recoveries for AS residues spiked in tobacco are higher than 95% for AS, 91% for ASN and 85% for ASX at levels of 0.5-10 ppm (w/w). The detection limit is 0.5 ppm for each of the target compounds.

摘要

描述了一种用于测定烟草中低ppm水平涕灭威（AS）及其亚砜（ASX）和砜（ASN）代谢物的筛查方法。烟草样品在环境条件下借助超声处理用甲醇进行萃取。提取物经过过滤，然后注入配备双柱后反应系统和荧光检测器的高效液相色谱仪中。在C18柱上进行色谱分离，以含有0.1%三乙醇胺的甲醇 - 乙腈 - 水混合物作为流动相。添加三乙醇胺以改善AS残留物的峰形，并减少残留硅烷醇与干扰物（主要是氨基酸和其他胺类）之间的不良相互作用。在0.5 - 10 ppm（w/w）水平下，添加到烟草中的AS残留物的平均回收率对于AS高于95%，对于ASN为91%，对于ASX为85%。每种目标化合物的检测限为0.5 ppm。