色谱

色谱 ›› 2012, Vol. 30 ›› Issue (02): 160-164.DOI: 10.3724/SP.J.1123.2011.10001

• 研究论文 • 上一篇    下一篇

高效液相色谱-串联质谱法检测玩具中5种香豆素类致敏性香味剂

杨荣静*, 卫碧文, 高欢, 于文佳   

  1. 上海出入境检验检疫局, 上海 200135
  • 收稿日期:2011-10-07 修回日期:2011-11-14 出版日期:2012-02-28 发布日期:2012-03-22
  • 通讯作者: 杨荣静,博士,工程师,主要从事玩具中有毒有害有机物的检测. Tel: (021)38620900,

Determination of five coumarins in toys by high performance liquid chromatography-tandem mass spectrometry

YANG Rongjing*, WEI Biwen, GAO Huan, YU Wenjia   

  1. Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China
  • Received:2011-10-07 Revised:2011-11-14 Online:2012-02-28 Published:2012-03-22

PDF

358

被引次数

15

摘要： 建立了一种简单、快速、准确测定玩具中香豆素、7-甲氧基香豆素、二氢香豆素、7-甲基香豆素、7-乙氧基-4-甲基香豆素5种香豆素类致敏性香味剂的检测方法。样品经四氢呋喃超声提取,提取液浓缩至近干,以25 mL甲醇 溶解残渣定容后进行高效液相色谱-串联质谱分析。色谱流动相为乙腈和0.1%乙酸水溶液,梯度洗脱,多反应监 测（MRM）模式进行定性和定量分析。5种目标物的工作曲线线性范围均为10～1 000 μg/L;除了二氢香豆素的定 量限（信噪比（S/N）>10）为5.0 μg/L外,其他化合物均为2.0 μg/L;在3种不同类型的样品中添加高、中、低水平的5种目标物标准品,其加标回收率为93.2%～105.8%,相对标准偏差为3.65%～8.27%。应用本方法对12种玩具和儿童用品样品进行了测试,其中9个样品中检出了香豆素类致敏性香味剂,有两个样品中香豆素和7-甲氧基香豆素的含量超过了欧盟玩具新指令的限量要求。

关键词: 高效液相色谱-串联质谱, 玩具, 香豆素, 致敏性香味剂

Abstract: A rapid analytical method for the determination of five coumarins （coumarin, 7-methoxycoumarin, dihydrocoumarin, 7-methyl coumarin and 7-ethoxy-4-methyl coumarin） in toys by high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） has been developed. After ultrasonic extraction in tetrahydrofuran, the samples were analyzed by HPLC-MS/MS in multi-reaction monitoring （MRM） mode. Acetonitrile and 0.1% acetic acid were used as the mobile phases with gradient elution. The linear ranges of calibration curves were 10~1000 μg/L, and the limits of quantification （LOQ） （S/N>10） were 2.0 μg/L for all the analytes, except that the LOQ for dihydrocoumarin was 5.0 μg/L. The recoveries of the five coumarins spiked in three types of samples were in the ranges of 93.2%~105.8%, 97.3%~ 103.2% and 96.8%~102.9%, with the relative standard deviations in the ranges of 4.35%~8.27%, 3.65%~6.73% and 4.03%~6.45%, respectively. The method was applied in the determination of 12 toy samples. The five analytes were found in 9 samples, and in some cases, the presence of quite high concentrations of these coumarins in the toys should be a matter of concern.

Key words: coumarins, fragrance allergens, toys, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)