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

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

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0.0013~0.42 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%。

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%.