色谱

色谱 ›› 2012, Vol. 30 ›› Issue (06): 596-601.DOI: 10.3724/SP.J.1123.2012.02013

• 研究论文 • 上一篇    下一篇

固相萃取-气相色谱-质谱法测定木制家具中氯酚类及菊酯类防腐剂

李海玉, 张庆*, 康苏媛, 吕庆, 白桦, 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:2012-02-09 修回日期:2012-03-29 出版日期:2012-06-28 发布日期:2012-06-20
  • 通讯作者: 张庆,博士,副研究员,主要研究方向为消费品安全. Tel: (010)85773355-2063, E-mail: njuzhangqing@caiq.gov.cn.
  • 基金资助:

    质检公益性行业科研专项(No. 201010013)和中国检验检疫科学研究院基本科研业务费专项资金项目(No. 2012JK018).

Determination of chlorophenol and pyrethroid preservatives in wooden furniture by solid phase extraction coupled with gas chromatography-mass spectrometry

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

  1. Institute of Industrial Product Inspection, Chinese Academy of Inspection and Quarantine, Beijing 100123, China
  • Received:2012-02-09 Revised:2012-03-29 Online:2012-06-28 Published:2012-06-20

PDF

333

被引次数

32

摘要： 建立了固相萃取-气相色谱-质谱(SPE-GC-MS)检测含氯酚类化合物(2,4-二氯苯酚、2,4,6-三氯苯酚、2,4,5-三氯苯酚、2,3,4,6-四氯苯酚、五氯苯酚、林丹)和菊酯类化合物(氯菊酯、氟氯氰菊酯、氯氰菊酯、溴氰菊酯)等10种木材防腐剂的方法。对家具样品采用超声萃取法、以甲醇为提取剂在室温下反复提取2次,提取液经浓缩后,加入碳酸钾和乙酰酐衍生化,将衍生化后的溶液通过Oasis HLB固相萃取柱净化,用乙酸乙酯洗脱并收集检测。采用该方法实现了家具中10种木材防腐剂的分离检测,该方法中氯酚类防腐剂定量限为1 mg/kg、菊酯类防腐剂定量限为5 mg/kg,平均回收率为76.0%～108.8%。应用该方法对市场上销售的木制家具进行了检测,在部分家具中检出含有少量林丹。实验结果证明,该方法准确、灵敏,可有效地应用于木制家具中防腐剂的实际检验工作中。

关键词: 固相萃取, 菊酯类防腐剂, 氯酚类防腐剂, 木制家具, 气相色谱-质谱法

Abstract: A method for the determination of 10 wood preservatives of chlorophenols (2,4-dichlorophenol, 2,4,6-trichlorophenol, 2,4,5-trichlorophenol, 2,3,4,6-tetrachlorophenol, pentachlorophenol, lindane) and pyrethroids (permethrin, cyfluthrin, cypermethrin, deltamethrin) in furniture by solid phase extraction (SPE) coupled with gas chromatography-mass spectrometry (GC-MS) was developed. The furniture samples were extracted twice by ultrasonic extraction in methanol. The extract was then evaporated and acetylated by the acetic anhydride and potassium carbonate. Finally the reaction solution was purified by Oasis HLB SPE column. The wood preservatives were eluted by ethyl acetate and collected for analysis by GC-MS. The ten wood preservatives can be separated and determined successfully by this method. Under the optimized conditions, the detection limits of the six chlorophenol compounds were 1 mg/kg, and the four pyrethroid compounds were 5 mg/kg, and the spiked recoveries of the 10 wood preservatives in samples were in the range of 76.0%-108.8%. Forty commercial wooden furniture samples were tested and lindane was found in some samples. The results showed that the method is accurate, rapid and sensitive. It can be effectively used to analyze the wood preservatives in wooden furniture.

Key words: chlorophenol preservative, gas chromatography-mass spectrometry (GC-MS), pyrethroid preservative, wooden furniture, solid phase extraction (SPE)