摘要
建立了固相萃取-气相色谱-串联质谱法（SPE-GC-MS/MS）同时测定木制儿童用品中氯酚类化合物和菊酯类化合物等10种木材防腐剂.采用甲醇溶剂提取,乙酸酐试剂衍生、固相萃取净化后,经HP-5MS色谱柱（30 m×0.25 mm×0.25 μm）分离,串联质谱在多反应离子监测模式（MRM）下进行检测,内标法定量.同时,考察了多种实验参数对检测结果的影响,并进行方法验证.结果表明,该方法对于复杂基质的木材样品中目标物的检测具有良好的选择性与灵敏度.对于不同物质的定量限（LOQ）在0.002 5～0.2 mg/kg之间,线性范围为0.002 5～25 mg/kg,低、中、高3个添加水平的平均回收率在85.2％～100.1％之间,日内精密度（RSD,n=6）在0.6％～9.1％之间,日间精密度（RSD,n=6）在2.3％～7.2％之间.将该方法应用于实际样品抽查中,发现了多种木材防腐剂的残留.
Ten kinds of wood preservatives of chlorophenols and pyrethroids in wooden children＇s products were determined simultaneously using solid phase extraction coupled with gas chromatography-tandem mass spectrometry （SPE-GC-MS/MS）.The sample was ultrasonically extracted with methanol.The extract was evaporated and then derivatised with acetic anhydride.Finally the solution was purified using Oasis HLB SPE column.The separations were performed on an Agilent HP-SMS column （30 m×0.25 mm×0.25 μm）,then were determined by MS/MS and quantified by internal standard method.Procedures for extraction and purification were carefully optimized.The method was proved to be linear over a wide range of concentrations for all analytes with the correlation coefficients greater than 0.999 3.Limits of detection （LODs） and limits of quantification （LOQs） are in the range of 0.001-0.05 mg/kg and 0.002 5-0.2 mg/kg,respectively.Average recoveries of target compounds （spiked at three concentration levels） are in the range of 85.2％-100.1％.Intraday and interday repeatability （RSD,n=6） of the proposed method are vary of 0.6％-9.1％ and 2.3％-7.2％,respectively.The proposed method was used to monitor preservatives in commercial wooden toys,and some preservatives were found.
出处
《质谱学报》
EI
CAS
CSCD
北大核心
2013年第6期321-329,共9页
Journal of Chinese Mass Spectrometry Society
基金
科技支撑计划(2013BAK04B03)
质检公益性行业科研专项(201310057)
中国检验检疫科学研究院基本科研业务费专项(2012JK018)资助
关键词
气相色谱-串联质谱法
木材防腐剂
固相萃取
木制儿童用品
gas chromatography-tandem mass spectrometry
wood preservatives
solid phase extraction
wooden children＇s products
