色谱

色谱 ›› 2012, Vol. 30 ›› Issue (05): 480-486.DOI: 10.3724/SP.J.1123.2011.12005

• 研究论文 • 上一篇    下一篇

气相色谱-离子阱质谱联用测定玩具中21种致敏性芳香剂

吕庆, 张庆*, 白桦, 李海玉, 康苏媛, 王超   

  1. 中国检验检疫科学研究院工业品检验研究所, 北京 100123
  • 收稿日期:2011-12-02 修回日期:2012-02-09 出版日期:2012-05-28 发布日期:2012-06-07
  • 通讯作者: 张庆,博士,副研究员,研究方向为消费品安全分析. E-mail: njuzhangqing@yahoo.com.cn.
  • 基金资助:

    质检公益性行业科研专项计划项目(No. 20100019)和中国检验检疫科学研究院基本科研业务专项基金项目(No.2010JK013).

Determination of 21 fragrance allergens in toys by gas chromatography-ion trap mass spectrometry

LV Qing, ZHANG Qing*, BAI Hua, LI Haiyu, KANG Suyuan, WANG Chao   

  1. Institute of Industrial Product Inspection, Chinese Academy of Inspection and Quarantine, Beijing 100123, China
  • Received:2011-12-02 Revised:2012-02-09 Online:2012-05-28 Published:2012-06-07

PDF

342

被引次数

30

摘要： 建立了气相色谱-离子阱质谱联用测定布绒、贴纸和塑料玩具中苯甲醇等21种致敏性芳香剂的方法。对于布绒和贴纸玩具样品,采用丙酮超声振荡提取20 min后过0.45 μm滤膜,经HP-1MS色谱柱(50 m×0.2 mm×0.5 μm)分离,离子阱质谱检测。对于塑料玩具样品,采取溶解-沉淀方式提取,经Envi-carb石墨化碳固相萃取小柱净化,旋蒸、氮吹浓缩,过0.45 μm滤膜后进行测定,外标法定量。方法对不同物质的定量限(LOQ)为0.02～40 mg/kg,线性范围为0.002～50 mg/L,低、中、高3个添加水平的平均回收率为82.2%～110.8%,相对标准偏差(RSD)为0.6%～10.5%。该方法准确、灵敏,可用于玩具中苯甲醇等21种致敏性芳香剂含量的检测。

关键词: 气相色谱-离子阱质谱, 玩具, 致敏性芳香剂

Abstract: A method of gas chromatography-ion trap mass spectrometry (GC-IT-MS) was developed for the determination of 21 fragrance allergens in sticker toys, plush toys and plastic toys. The experimental conditions, such as sample pretreatment conditions, and the analytical conditions of GC-IT-MS, were optimized. The sticker toy samples and plush toy samples were extracted with acetone by ultrasonic wave, and the extracts were separated on an Agilent HP-1MS column (50 m×0.2 mm×0.5 μm), then determined by IT-MS and quantified by external standard method. The plastic toy samples were extracted by the dissolution-precipitation approach, cleaned up with an Envi-carb solid phase extraction column and concentrated by rotary evaporation and nitrogen blowing, then determined by GC-IT-MS and quantified by external standard method. The calibration curves showed good linearity in the range of 0.002~50 mg/L with the correlation coefficients greater than 0.9968. The limits of quantification (LOQ, S/N＞10) were 0.02~40 mg/kg. The average recoveries of the target compounds spiked in the sample at three concentration levels were in the range of 82.2%~110.8% with the relative standard deviations (RSDs) of 0.6%~10.5%. These results show that this method is accurate and sensitive for the qualitative and quantitative determination of the 21 fragrance allergens in the 3 types of toys.

Key words: fragrance allergens, toys, gas chromatography-ion trap mass spectrometry (GC-IT-MS)

中图分类号: