Li Haiyu, Zhang Qing, Kang Suyuan, Lü Qing, Bai Hua, Wang Chao
Institute of Industrial Product Inspection, Chinese Academy of Inspection and Quarantine, Beijing 100123, China.
Se Pu. 2012 Jun;30(6):596-601. doi: 10.3724/sp.j.1123.2012.02013.
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, delta-methrin) 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.
建立了一种采用固相萃取（SPE）结合气相色谱 - 质谱联用（GC - MS）测定家具中10种木材防腐剂的方法，这些防腐剂包括氯酚类（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）和拟除虫菊酯类（氯菊酯、氟氯氰菊酯、氯氰菊酯、溴氰菊酯）。家具样品用甲醇超声萃取两次。萃取液经蒸发后，用乙酸酐和碳酸钾进行乙酰化反应。最后，反应溶液通过Oasis HLB固相萃取柱进行净化。木材防腐剂用乙酸乙酯洗脱并收集，用于GC - MS分析。采用该方法可成功分离并测定这10种木材防腐剂。在优化条件下，6种氯酚类化合物的检出限为1 mg/kg，4种拟除虫菊酯类化合物的检出限为5 mg/kg，样品中10种木材防腐剂的加标回收率在76.0% - 108.8%范围内。对40个商用木制家具样品进行了检测，部分样品中检测出了林丹。结果表明，该方法准确、快速、灵敏，可有效用于分析木制家具中的木材防腐剂。
