摘要
本研究通过不同溶剂索氏提取和凝胶渗透色谱(GPC)净化条件的比较研究,建立了基于自动索氏抽提-凝胶渗透色谱(GPC)-气相色谱/质谱法同时测定渔业养殖环境中养殖水(直接溶剂萃取,无需索氏抽提)、底泥及草鱼、罗氏沼虾、中华绒螯蟹等水产品中16种多环芳烃(PAHs)残留量的方法。样品中的多环芳烃由环己烷∶丙酮(体积比1∶1)、环己烷∶二氯甲烷(体积比1∶1)、丙酮∶二氯甲烷(体积比1∶1)混合溶剂索氏提取,经GPC净化后,通过DB35-MS毛细管色谱柱分离,采用电子轰击源选择反应监测模式进行质谱分析,以内标法定量。结果显示,16种渔业养殖环境平均检出限为0.017~0.171μg/kg,测定下限为0.051μg/kg,底泥的加标回收率达到52.4%~110.7%,相对标准偏差为0.64%~8.94%,养殖用水的加标回收率达到74.1%~116.7%,相对标准偏差为0.52%~8.91%,水产品的加标回收率达到70.3%~126.4%,相对标准偏差为0.14%~8.91%。表明本研究方法满足渔业养殖环境(养殖用水、底泥)及水产品中PAHs的含量测定。
Based on automatic Soxhlet extraction-gel permeation chromatography(GPC)-gas chromatography/mass spectrometry(GC/MS),a method has been developed for the determination of 16 polycyclic aromatic hydrocarbons(PAHs)in aquaculture water,sediment and aquatic products(grass carp,Macrobrachium rosenbergii,Eriocheir sinensis)by comparing different Solvent soxhlet extraction and GPC purification conditions.In addition,the aquaculture water was extracted directly by solvent without Soxhlet extraction.The sample were extracted in automated Soxhlet extraction with cyclohexane∶acetone(volume ratio 1∶1),cyclohexane∶methylene chloride(volume ratio 1∶1),and acetone∶methylene chloride(volume ratio 1∶1)after injecting into GPC to purifying.The purified samples were separated by DB35-MS capillary chromatographic column.The electron bombardment source selection reaction monitoring model was used for mass spectrometry analysis,and internal standard method was used for quantitative analysis.The result showed that the average detection limit of 16 PAHs in aquaculture environments ranged from 0.017μg/kg to 0.171μg/kg,and the lower limit of measurement was 0.051μg/kg.The average spiked recovery rates of sedimen were in the range of 52.4%-110.7%,and the relative standard deviation was in the range of 0.64%-8.94%.The average spiked recovery rates of aquaculture water were in the range of 74.1%-116.7%,the relative standard deviation was in the range of 0.52%-8.91%.The average spiked recovery rates of aquatic products were in the range of 70.3%-126.4%,and the relative standard deviation was in the range of 0.14%-8.91%,respectively.The method could be used for the determination of PAHs residues in aquaculture environment(including water and mud)and aquatic products.
作者
徐志华
朱晓华
葛筱琴
耿雪冰
刘崇万
沈美芳
XU Zhi-hua;ZHU Xiao-hua;GE Xiao-qin;GENG Xue-bing;LIU Chong-wan;SHEN Mei-fang(Freshwater Fisheries Research Institute of Jiangsu Province,Nanjing 210017,China;Fishery Analysis&Testing Center of Jiangsu Province/Quality Control&Inspection Center for Domestic Fishery Products,Ministry of Agriculture and Rural Affairs(Nanjing),Nanjing 210017,China)
出处
《江苏农业学报》
CSCD
北大核心
2019年第6期1459-1467,共9页
Jiangsu Journal of Agricultural Sciences
基金
江苏现代农业产业技术体系建设专项(JFRS-05)
江苏省农业科技自主创新基金项目[CX(18)2011]
关键词
渔业养殖环境
水产品
多环芳烃
气相色谱质谱法
凝胶渗透色谱
aquaculture environment
aquatic product
polycyclic aromatic hydrocarbons(PAHs)
gas chromatography/mass spectrometry
gel permeation chromatography
