标准及检测

液相色谱-串联质谱法测定水性涂料中5种异噻唑啉酮生物杀伤剂

  • 李广东
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  • 中海油常州涂料化工研究院有限公司,江苏常州 213016
李广东(1989—),男,工程师,主要从事涂料产品检测和标准化工作。

收稿日期: 2019-07-01

  修回日期: 2019-10-18

  网络出版日期: 2019-12-01

Determination of Five Isothiazolinone Biocides in Waterborne Coatings by LC-MS/MS

  • LI An-Dong
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  • CNOOC Changzhou Paint & Coatings Industry Research Institute Co.,Ltd., Changzhou, Jiangsu 213016,China

Received date: 2019-07-01

  Revised date: 2019-10-18

  Online published: 2019-12-01

摘要

建立并优化了水性涂料中 5种异噻唑啉酮生物杀伤剂的检测方法。采用 Optimizer优化软件优化了子离子、碎裂电压和碰撞能量等参数。考察了流动相中甲酸和乙酸铵的含量、流动相梯度洗脱程序、毛细管电压、干燥气流速、雾化器压力、加速电压、干燥气温度等参数对质谱响应的影响。样品用体积分数为 50%的甲醇水溶液或甲醇于容量瓶中经稀释、搅拌和超声提取,提取液经离心分离、过滤膜后,用液相色谱 -串联质谱检测。实验结果表明:在稀释最低 98倍的浓度范围内, 5种异噻唑啉酮的标准曲线线性关系良好,方法的检出限为 0. 001 3~0. 42 mg/kg。空白样品加标回收率在 86. 73%~93. 60%之间,相对标准偏差为 2. 3%~5. 8%。

本文引用格式

李广东 . 液相色谱-串联质谱法测定水性涂料中5种异噻唑啉酮生物杀伤剂[J]. 涂料工业, 2019 , 49(12) : 54 -61 . DOI: 10.12020/j.issn.0253-4312.2019.12.54

Abstract

An optimized method was established for determination of 5 isothiazolinone biocides in waterborne coatings. The Optimizer software was used to optimize the parameters such as product ion,fragmentation voltage and collision energy. The influences of the parameters of ammonium acetate and formic acid in eluents,gradients,capillary voltage,dry gas flow rate and nebulizer pressure,acceleration voltage,temperature of dry gas on the mass spectral response was investigated. The samples were diluted with a mixture of water and methanol(1∶1 by volume)or methanol,and homogenized in one-mark volumetric flasks. The extraction was performed in an ultrasonic generator. The extract solution was separated by centrifuge and filtrated. The sample solutions were detected by liquid chromatography-tandem mass spectrometry. The experimental results showed that the linear curve of the 5 isothiazolinones indicated a good linear relationship in the concentration range of more than 98 times dilution. The detection limit of the method was 0. 0013 mg / kg to 0. 42 mg / kg. The recoveries of spiked samples were between 86. 73%and 93. 60%,and the relative standard deviations were 2. 3%~5. 8%.

参考文献

[1] HERMAN A,AERTS O,DE MONTJOYE L,et al.Isothiazolinone derivatives and allergic contact dermatitis:a review and update[J]. Journal of the European Academy of Dermatology and Venereology,2018,33(2).
[2]LINQB,WANG T J,SONG H,et al.Analysis of isothiazolinone biocides in paper for food packaging by ultra -high-performance liquid chromatography-tandem mass spectrometry[J].Food Additives & Contaminants:Part A, 2010, 27(12):1775-1781
[3]全国涂料和颜料标准化技术委员会 .绿色产品评价 涂料: GB/T 35602—2017[S].北京:中国标准出版社, 2018.
[4]ALVAREZ-RIVERA G,DAGNAC T,LORES M,et al. Determination of isothiazolinone preservatives in cosmetics and household products by matrix solid-phase dispersion followed by high-performance liquid chromatography-tandem mass spectrometry[J].[J].Journal of Chromatography A, 2012, 1270:41-50
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