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高效液相色谱-串联质谱法同时测定儿童彩泥类造型玩具中3种异噻唑啉酮类防腐剂
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王瑾,任洁芳,张东雷,周敏,李祖光,张慧敏 1.浙江省产品质量安全检测研究院
2.浙江工业大学化学工程学院 
基金项目:浙江省质量技术监督系统科研计划项目(20180101)
中文摘要:建立了儿童彩泥类造型玩具中异噻唑啉酮类防腐剂(2-甲基-4-异噻唑啉 3-酮(MI)、5-氯 2-甲基 4-异噻唑啉 3-酮(CMI)和1,2 苯并异噻唑啉-3-酮(BIT))的高效液相色谱-串联质谱(HPLC-MS/MS)测定方法。样品经甲醇超声提取、离心、过滤后,采用KinetexC18色谱柱(100 mm×3 mm,2.6 μm)进行分离,流动相为甲醇-水,梯度洗脱,流速300 μL/min。在多反应监测(MRM)模式下定性,外标法定量。结果表明,3种异噻唑啉酮类防腐剂在1.0~100.0 μg/L质量浓度范围内线性关系良好(r≥0.999 0),3种化合物的平均回收率为80.2%~109%,相对标准偏差(RSD,n=5)为1.3%~7.0%。MI、CMI和BIT的检出限(LOD)分别为10、10、20 μg/kg,定量下限(LOQ)分别为30、30、60 μg/kg。
中文关键词:高效液相色谱-串联质谱  异噻唑啉酮类防腐剂  儿童彩泥类造型玩具
 
Determination of Three Isothiazolinone Preservatives in Childrens Color Clay Modeling Toys by High Performance Liquid Chromatography-Tandem Mass Spectrometry
Abstract:A rapid analytical method was developed for the determination of three isothiazolinone reservatives,i.e2-methyl-4-isothiazoline-3-one(MI),5-chloro-2-methyl-4-isothiazoline-3-one(CMI) and 1,2-benzothiazol-3-one(BIT) in children's color clay modeling toys by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The sample was ultrasonically extracted with methanol,then filtrated after centrifugation,and finally separated on a Kinetex C18 column(100 mm×3 mm,2.6 μm) by gradient elution with methanol and water as mobile phases at a flow rate of 300 μL/min.The sample was analyzed by HPLC-MS/MS in multiple reaction monitoring(MRM) mode,and quantified by the external standard method.Results showed that there were good linear relationships for three analytes in the concentration range of 1.0-100.0 μg/L with correlation coefficients(r) not less than 0.999 0.Average recoveries for the analytes ranged from 80.2% to 109%,with relative standard deviations(RSD,n=5) of 1.3%-7.0%.The limits of detection(LOD) for MI,CMI and BIT were 10,10 and 20 μg/kg,and the limits of quantitation(LOQ) were 30,30 and 60 μg/kg,respectively.
Key Words:high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)  isothiazolinone preservatives  childrens color clay modeling toys
引用本文:王瑾,任洁芳,张东雷,周敏,李祖光,张慧敏.高效液相色谱-串联质谱法同时测定儿童彩泥类造型玩具中3种异噻唑啉酮类防腐剂[J].分析测试学报,2019,38(11):1384-1388.
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