摘要
为准确测定烟用纸张中异噻唑啉酮类杀菌剂的残留量，建立了一种液相色谱-串联质谱法（LC-MS/MS）快速测定烟用纸张中3种异噻唑啉酮类杀菌剂[2-甲基-4-异噻唑啉-3-酮（MI）、5-氯-2-甲基-4-异噻唑啉-3-酮（CMI）和1，2-苯并异噻唑啉-3-酮（BIT）]的方法。样品经甲醇超声提取、离心、过滤后，用氟苯基柱，以甲醇-水为流动相进行分离，采用LC-MS/MS在多反应监测模式下测定，内标法定量。结果表明：方法加标回收率在89.1%～110.8%之间，相对标准偏差≤7.1%，检出限为0.014～0.018 mg/kg，定量限为0.045～0.059 mg/kg。该方法简单、准确，适用于烟用纸张中痕量异噻唑啉酮类杀菌剂的定性和定量分析。
In order to accurately determine the residues of isothiazolinone biocides in paper for cigarette （cigarette paper,plug wrap,inner liner and tipping paper）,a rapid liquid chromatography-tandem mass spectrometry（LC-MS/MS）method for determining three isothiazolinone biocides （2-methyl-4-isothiazolin-3-one,5-chloro-2-methyl-4-isothiazolin-3-one and 1,2-benzylisothiazolin-3-one）was developed. The paper sample was ultrasonically extracted with methanol, then the extract was centrifuged, the supernatant liquid was filtrated and then injected into LC-MS/MS and separated in a fluorine phenyl column by using methanol-water as mobile phase. The analytes were detected by LC-MS/MS under multiple reaction monitoring mode and quantified by an internal standard method. The results displayed that the recoveries of the proposed method ranged from 89.1% to 110.8%,and the relative standard deviations were not higher than 7.1% for all analytes. The LODs and LOQs were 0.014-0.018 and 0.045-0.059 mg/kg,respectively. This method is simple,accurate and suitable for the qualitative and quantitative analysis of trace isothiazolinone biocides in paper for cigarette.
出处
《烟草科技》
EI
CAS
CSCD
北大核心
2016年第8期57-63,共7页
Tobacco Science & Technology
基金
国家烟草专卖局标准项目"烟用材料中异噻唑啉酮类杀菌剂残留量及迁移量分析研究"(2014QB011)
关键词
液相色谱-串联质谱法
烟用纸张
异噻唑啉酮类杀菌剂
Liquid chromatography-tandem mass spectrometry
Paper for cigarette
Isothiazolinone biocide
