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.
Chinese Journal of Pest Control
Gas chromatography-tandem mass spectrometry