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

Determination of 3 isothiazolinone preservatives in toys using liquid chromatography-tandem mass spectrometry

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-酮)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 chromatographytandem 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 μg/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 EN7111-2005.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.