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-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.
出处
《色谱》
CAS
CSCD
北大核心
2011年第6期513-516,共4页
Chinese Journal of Chromatography
关键词
液相色谱-串联质谱
异噻唑啉酮
防腐剂
玩具
liquid chromatography-tandem mass spectrometry(LC-MS/MS)
isothiazolinones
preservatives
toys