液相色谱-串联质谱法检测玩具中的3种异噻唑啉酮类防腐剂

摘要

建立了液相色谱-串联质谱快速测定玩具中异噻唑啉酮类防腐剂(2-甲基-4-异噻唑啉-3-酮、5-氯-2-甲基-4-异噻唑啉-3-酮和1,2-苯并异噻唑啉-3-酬)的分析方法.样品经去离子水超声提取后进行液相色谱-串联质谱分析.色谱流动相为甲醇-水(15：85,v/v),等度洗脱,在选择反应监测(SRM)模式下定性和定量分析.3种被分析物的工作曲线线性范围均为2.0～1 000μg/L,方法的定量限(信噪比大于10)为0.04 mg/kg,灵敏度优于欧盟玩具协调标准EN71-11-2005中推荐的方法.两种类型玩具样品中的加标回收率分别为95.9％～105.2％和94.7％～102.8％,精密度分别为3.04％～4.96％和2.36％～4.79％.应用本方法对10种玩具样品进行了测试,结果完全能满足欧盟玩具协调标准EN71-9-2005对玩具中异噻唑啉酮类防腐剂的检测要求.%A rapid analytical method for the determination of 3 isothiazolinone preservatives (2-methyl-4-isothiazolin-3-one, 5-chloro-2-methyl-4-isothiazolin-3-one and 1,2-benzylisothiazolin-3-one) in toys using liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed. After ultrasonic extraction with water, the analytes in the sample were separated and analyzed by LC-MS/MS under the isocratic elution of methanol and water (15: 85 , v/v) and in selected-reaction monitoring (SRM) mode. The linear ranges of calibration curves for the 3 analytes were 2. 0 - 1 000 jjig/L. The limit of quantification was 0. 04 mg/kg for all the 3 analytes, which was lower than that of the method recommended by the European Toy Safety Directive in EN71-11-2005. The recoveries of the spiked standards in the two.toy samples were 95. 9% - 105. 2% and 94. 7% - 102. 8% with the relative standard deviation ranges from 3. 04% to 4. 96% and from 2. 36% to 4. 79%, respectively. The method was applied in the determination of 10 toy samples, and the results can meet the requirements of the European Toy Safety Directive in EN71-9-2005 for the determination of isothiazolinones in toys.