摘要
为了快速检测和确证人参中五氯硝基苯及其代谓十物的残留量，建立了气相色谱／离子阱串联质谱法（GC-MS／MS）同时测定人参中五氯硝基苯（PCNB）及其2种代谢产物五氯苯胺（PCA）和甲基五氯苯硫醚（PC-TA）残留分析方法。样品用正己烷均质提取，弗洛里硅土固相萃取柱（Florisil-SPE）净化，采用GC-MS／MS多反应监测模式（MRM）检测，外标法定量。在人参中五氯硝基苯和五氯苯胺检出限均为1 ng／g，甲基五氯苯硫醚为0.1 ng／g；在0．01～0．5μg／g添加范围内，五氯硝基苯、五氯苯胺和甲基五氯苯硫醚的添加回收率分别为82．2％～89．4％、82．3％～84．7％和84．1％～88．5％；相对标准偏差均小于8．6％；检出限保持在0．1～1 ng／g之间（信噪比10）。
For validation and fast determination of residues of pentachloronitrobenzene and its metabolites in ginseng, the residual method was established to determinate pentachloronitrobenzene （PCNB） , pentachloroaniline（PCA） and pentaehlorothioanisole （PCTA） in ginseng by gas chromatography-ion trap tandem mass spectrometry （GC-MS/MS）. Homogenized ginseng sample were extracted by n-haxene, cleaned up by florisil solid phase extraction （LC-Florisil）cartridge. Identification was carried out by GC-MS/MS in multiple reaction monitoring mode. The limit of detection of PCNB and PCA in ginseng was both 1 μg/kg, and that of PCTA was 0.1 μg/kg. The recoveries of PCNB, PCA and PCTA in ginseng were 82.2% - 89.4% , 82.3% - 84.7% and 84. 1% -88.5% ,respectively, at spiked levels of 0.01 μg/g-0.5 μg/g. The relative standard deviations （RSD） were less than 8.6%, and the limit of detection （LOD） was defined in terms of 10 times baseline noise, varied from 0.1 ng/g to 1 ng/g, depending on the compound.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2008年第12期1716-1720,共5页
Chinese Journal of Analytical Chemistry
基金
支撑计划粮食分产工程(No.2006BAD02A16)资助项目
关键词
气相色谱/离子阱串联质谱法
五氯硝基苯
五氯苯胺
甲基五氯苯硫醚
多反应监测
人参
Gas chromatography-ion trap tandem sepectrometry, pentachloronitrobenzene, pentachloroaniline, pentachlorothioanisole, multiple reaction monitoring, ginseng
