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基质固相分散萃取-气相色谱法同时检测人参中五氯硝基苯及其代谢物残留
Simultaneous Determination of Pentachloronitrobenzene Residue and Its Metabolites Pentachloroaniline and Pentachlorothioanisole in Ginseng Based on Matrix Solid Phase Dispersion and Gas Chromatography
【摘要】 采用基质固相分散萃取-气相色谱(MSPD-GC)技术,建立了人参中五氯硝基苯(PCNB)及其代谢物五氯苯胺(PCA)和甲基五氯苯基硫醚(PCTA)残留的多残留分析方法。将人参样品与弗罗里硅土(m/m,1∶2)充分研磨5min后装入10mL玻璃注射器内,通过正己烷∶丙酮(V/V,5∶5)混合溶液洗脱实现了人参中五氯硝基苯及其代谢物的同时提取和净化。结果表明,应用该方法测定人参中五氯硝基苯、五氯苯胺及甲基五氯苯基硫醚,回收率为89.41%~104.42%,相对标准偏差为3.73%~7.43%,五氯硝基苯及其代谢物的方法检出限均小于2μg·kg-1。
【Abstract】 An effective and simple method for simultaneous determination of pentachloronitrobenzene(PCNB)residue and its metabolites pentachloroaniline(PCA), pentachlorothioanisole(PCTA)in ginseng was developed based on matrix solid-phase dispersion and gas chro- matography. Dry ground ginseng samples and florisil sorben(t1∶2)were homogenized in a mortar for 5 min and then packed into a 10 mL of glass syringe. Eluted with hexane/acetone=5∶5(V/V)solution, pentachloronitrobenzene and its metabolites were simultaneously extracted and cleaned up. The qualitative and the quantitative analysis of samples was accomplished using gas chromatography with ECD(electronic cap- ture detector). The average recovery and relative standard deviation of PCNB, PCA and PCTA in ginseng at the spiked levels of 0.01, 0.05 and 0.1 mg·kg-1 was within 89.41%~104.42% and 3.73%~7.43% respectively. The limits of detection(LOD)of the method were 1.88, 1.50, 1.25 μg·kg-1 for PCNB, PCA and PCTA respectively. The proposed method was successfully applied to the determination of PCNB and its metabolites PCA and PCTA in ginseng with satisfactory results.
【Key words】 MSPD-GC; ginseng; residues; pentachloronitrobenzene; metabolites;
- 【文献出处】 农业环境科学学报 ,Journal of Agro-Environment Science , 编辑部邮箱 ,2009年01期
- 【分类号】R284
- 【被引频次】38
- 【下载频次】497