超高效液相串联质谱法测定水基胶中3种异噻唑啉酮类杀菌剂
Determination of 3 Isothiazolinone Fungicides in Water-based Adhesives by Ultra-performance Liquid Chromatography-tandem Mass Spectrometry
牛恩利 1孟倩 1毛宁 1江澜 1张红玉1
作者信息
- 1. 甘肃烟草工业有限责任公司技术研发中心,甘肃 兰州 730050
- 折叠
摘要
应用超高效液相串联质谱法(UPLC-MS/MS)快速测定水基胶中 2-甲基-3(2H)-异噻唑啉酮(MI)、5-氯-2-甲基-2H-异噻唑-3-酮(CMI)、1,2-苯并异噻唑基-3(2H)-酮(BIT)3 种异噻唑啉酮类杀菌剂的含量,前处理以水为分散剂、甲醇为萃取剂、超声 40 min进行提取目标化合物.采用多反应监测(MRM)技术,使用正离子扫描、多通道、分时段采集模式对目标化合物进行分析,3种同位素内标法定量.得到3种化合物的线性方程及相关系数,线性相关系数的范围为0.9991~0.9999,方法检出限为 0.06~0.10 mg·kg-1,定量限为0.21~0.32 mg·kg-1,各目标化合物的回收率在89.1%~103.5%,相对标准偏差(n=7)小于3.4%.该方法前处理简单、回收率高、重复性好,能够满足水基胶中3 种异噻唑啉酮类杀菌剂的快速检测需求.
Abstract
A method was developed for rapid determination of 2-methyl-4-isothiazolin-3-one(MI),5-chloro-2-methyl-4-isothiazolin-3-one(CMI),1,2-benzylisothiazolin-3-one(BIT)3 isothiazolinone fungicides in water-based adhesives using ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The pre-treatment used water as the dispersant and methanol as the extractant,and the target compound was extracted by ultrasound for 40 min.multiple reaction The monitoring(MRM)technology,positive scan mode,multi-channel,time-phased were used to analyse target compounds.3 isotope internal standard method were choiced for Quantitative analysis.The calibration curves of 3 compounds with correlation coefficients were in the range of 0.9991~0.9999,The limits of detection of the method for target compounds ranged from 0.06 to 0.10 mg·kg-1,the limits of quantitation varied from 0.21 to 0.32 mg·kg-1,The recoveries of target compounds ranged from 89.1% to 103.5% with relative standard deviations(RSDs,n=7) was less than 3.4%.This method had simple pre-treatment,high recovery rate and good repeatability,and could meet the rapid detection requirements of 3 isothiazolinone fungicides in water-based adhesives.
关键词
超高效液相串联质谱法/异噻唑啉酮类/杀菌剂/多反应监测/内标法Key words
UPLC-MS/MS/isothiazolinone/fungicides/MRM/internal standard引用本文复制引用
出版年
2024