气相色谱-负离子化学源-质谱法分析茶叶中5种多溴联苯醚  

Determination of five polybrominated diphenyl ethers in tea leaves by gas chromatography-mass spectrometry-negative chemical ionization

作　　者：林竹光[1] 马玉[1] 涂逢樟[1] 陈美瑜[1] 孙若男[1] 张莉莉[1] 李小波[1] 

机构地区：[1]厦门大学化学化工学院化学系现代分析科学教育部重点实验室,厦门361005

出　　处：《分析试验室》2007年第6期88-92,共5页Chinese Journal of Analysis Laboratory

摘　　要：将气相色谱-负离子化学源-质谱法（GC-NCI-MS）应用于快速分析茶叶中5种多溴联苯醚残留量.茶叶样品以正己烷作为提取剂,采用超声辅助提取法,提取液经中性氧化铝和Florisil硅藻土层析柱净化和正己烷洗脱后,以PCB-103为内标物和GC-NCI-MS的选择离子监测方式（SIM）进行定性与定量分析.5种多溴联苯醚的平均加标回收率为70.9%～81.7%,相对标准偏差为6.9%～11.0%,方法检出限小于0.12 μg/kg,线性范围为0.1～500 μg/kg,相关系数都大于0.9990.所分析的8种茶叶样品中6种含有微量的PBDE-47,1种茶叶样品含有微量的PBDE-99.A rapid method based on ultrasonic extraction was developed for the determination of five polybrominated diphenyl ethers in tea leaves. Hexane was used as the extraction solvent and elution solvent, after the extraction was cleaned by the cartridge filling with alumina and Florisil, the analysis of samples was accomplished using gas chromatography with negative chemical ionization mass spectrometric detection （GC-NCI-MS） in the selected ion monitoring mode （SIM）, and with PCB-103 as internal standard（IS）. The average recoveries of the standard samples spiked ranged from 70.9% to 81.7% with relative standard deviation between 6.9 and 11.0% for the five different polybrominated diphenyl ethers （PBDEs）, and the detection limit of the method was smaller than 0.12 μg/kg. The lineer range is from 0.1 to 500μg/kg, and the correlation coefficients were larger than 0.9990. Six out of the eight detenninated tea leaves had PBDE-47, and one had PBDE-99.

关 键 词：GC-NCI-MS 茶叶 多溴联苯醚 残留检测 

分 类 号：O657.63[理学—分析化学]