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气相色谱-三重四级杆串联质谱测定动物组织中五氯酚残留

Determination of residual pentachlorophenol in animal tissues by gas chromatography-tandem mass spectrometry
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摘要 目的建立一种固相萃取-气相色谱-串联质谱测定动物组织中五氯酚残留的方法,并对市售的动物组织中五氯酚残留量进行调查。方法样品经匀浆提取,离心,氮吹复溶,SLC固相萃取柱净化,净化液氮吹后加乙酸酐吡啶衍生,正己烷提取,上机测定,内标法定量。结果采用多反应监测模式(MRM)测定,并优化了色谱质谱条件。比较了50%硫酸和5%三氯乙酸的酸化提取效果,选择5%三氯乙酸作为萃取条件。方法的检测限为0. 05μg/kg,线性相关系数r=0. 9 996,加标回收率在97. 6%~102. 0%之间,相对标准偏差<5%。使用本法测定了市售60份动物组织样品,阳性检出率达到8. 3%。结论本方法降低了因操作、乳化和衍生等前处理变化而造成的影响,增强方法的可操作性、准确性和稳定性。五氯酚钠为禁止使用兽药,阳性检出的样品可能源于兽药滥用或者饲养环境污染。 Objective To establish a gas chromatography-tandem mass spectrometry analytic method for the determination of residual pentachlorophenol in animal tissues,and to investigate the residual pentachlorophenol in shell of market. Methods The sample was extracted by homogenization,centrifuged,re-dissolved by nitrogen,and purified by SLC solid phase extraction column. The purified liquid was blown with nitrogen and then extracted with acetic anhydride pyridine,extracted with n-hexane,determined by internal measurement,and quantified by internal standard method. Results The conditions of chromatography and mass spectrometry were optimized with multi-ion monitoring( MRM). The effects of 50% sulfuric acid solution and 5%trichloracetic acid as acidified extracted solution were compared. The extraction method of 5% trichloracetic acid was adopted. The detection limit of the method was 0. 05 μg/kg. The calibration curve of pentachlorophenol showed good linearity in the range of10. 0 ~ 200. 0 μg/L with correlation coefficient of 0. 9 996. the recovery of three spiking levels ranged from 97. 6% to 102. 0%,and the relative standard deviations( RSD) were < 5%. The method was used to determine 60 commercially available animal tissue samples. The prevalence of pentachlorophenol was 8. 3%. Conclusion The method reduces the influence of operation,emulsification and derivation process. The operability,accuracy and stability of the method gas have been greatly improved.
作者 曾涛 杨荣 邓芬芳 刘苗 于鸿 甘平胜 ZENG Tao;YANG Rong;DENG Fenfang;LIU Miao;YU Hong;GAN Pingsheng(Guangzhou Center for Disease Control and Prevention,Guangdong510440,China)
出处 《医学动物防制》 2019年第3期259-262,266共5页 Chinese Journal of Pest Control
基金 广州市医学重点学科建设项目(2017-2019-07).
关键词 五氯酚 固相萃取 气相色谱-串联质谱 食品安全 Pentachlorophenol Solid-phase extraction Gas chromatography-tandem mass spectrometry Food safety
作者简介 曾涛(1979-),男,主管技师,主要从事理化检验工作;通讯作者:杨荣,E-mail:237283784@qq.com.
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