色谱

色谱

• 研究论文 • 上一篇    下一篇

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

杨荣静1*, 卫碧文1, 于文佳1, 高欢1, 孙晓娟2   

  1. 1. 上海出入境检验检疫局, 上海 200135; 2. 赛默飞世尔科技(中国)有限公司, 上海 201206
  • 收稿日期:2011-02-14 修回日期:2011-03-23 出版日期:2011-06-28 发布日期:2011-07-25
  • 通讯作者: 杨荣静,博士,工程师,主要研究方向为玩具中有毒有害有机物的检测. Tel: (021)38620896

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

YANG Rongjing1*, WEI Biwen1, YU Wenjia1, GAO Huan1, SUN Xiaojuan2   

  1. 1. Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China; 2. ThermoFisher Scientific (China) Co., Shanghai 201206, China
  • Received:2011-02-14 Revised:2011-03-23 Online:2011-06-28 Published:2011-07-25

PDF

624

被引次数

56

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2.0～1 000 μg/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。

关键词: 防腐剂, 玩具, 液相色谱-串联质谱, 异噻唑啉酮

Abstract: The presence of isothiazolinones in toys is severely restricted in European Toy Safety Directive because of their allergenicity. A rapid analytical method for the determination of isothiazolinones (2-Methyl-4-isothiazolin-3-one, 5-Chloro-2-methyl-4-isothiazolin-3-one and 1,2-Benzylisothiazolin-3-one) in toys by liquid chromatography-tandem mass spectrometry has been developed. After ultrasonic extraction in water, samples were analyzed by LC-MS/MS. Methanol:water(15:85, V/V) isocratic elution was used as mobile phase. The linear ranges of calibration curves were 2.0 μg/L ~1 000 μg/L, and the limits of quantification for this method were 0.04 mg/kg for all the analytes employing selected-reaction monitoring (SRM) mass spectrometry. While for the recommended method in EN71-11:2005, the limit of quantification for 1,2-Benzylisothiazolin-3-one was 5 mg/kg, indicating that the sensitivity of this method was beyond that of the recommended method. The recoveries for two types of standard spiked samples were in the range of 95.9%~105.2% and 94.7%~102.8%, respectively, and the relative standard deviations ranged from 3.04% to 4.96% and 2.36% to 4.79%, respectively. The method was applied to ten toy samples, and the precision and sensitivity could meet the requirements of the determinations of isothiazolinones in toys in EN71-9:2005.

Key words: isothiazolinones, preservatives, toys, liquid chromatography-tandem mass spectrometry (LC-MS/MS)