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机构地区:[1]中国科学院水生生物研究所淡水生态与生物技术国家重点实验室 [2]湖北出入境检验检疫局技术中心,武汉430022
出 处:《分析科学学报》2008年第2期125-130,共6页Journal of Analytical Science
基 金:国家科技部973项目(No.2003CB415005);国家自然科学基金重大项目(No.40590390);中国科学院知识创新工程项目(KSCX-SW-128)
摘 要:研究了鮰鱼体内六溴环十二烷(HBCDs)异构体的浓度分布与生物累积特征。首先采用基质固相分散(MSPD)法,同位素稀释定量,高效液相色谱-电喷雾串联质谱(HPLC-ESI-MS/MS)检测技术,建立了渔业饲料和鱼体中α—HBCD、β—HBCD和γ—HBCD的分析方法。该法对α—HBCD、β—HBCD、γ-HBCD的回收率分别为80.7%~110.5%、80.1%~109.0%、86.9%~104.5%,其检出限分别为0.002、0.002、0.001ng/g。采用所建立的方法对25个渔业饲料样品和30个鱼样品进行分析,三种异构体在渔业饲料中的检出率均为16%,在鱼产品中的检出率分别为10%、6.67%和10%。鱼中HBCDs含量与渔业饲料中HBCDs含量的比值(生物累积因子)的结果为:α—HBCD,0.78;β—HBCD,0.45;γ—HBCD,1.08。对HBCDs在配对的渔业饲料与鱼中的相关关系进行了研究。Distribution and biomagnification characteristics of HBCDs in channel catfish have been studied in this paper. Isotope dilution high performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI-MS/MS) method has firstly been implemented to determine three diastereoisomers α-, β- and γ-HBCD in fish feeds and fish samples. Validation studies for the method on samples showed recoveries of 80.7%-110.5% for α-HBCD, 80.1%-109.0% for β-HBCD and 86.9%-104.5% for γ-HBCD at spiked levels of 0. 010, 0. 10 and 5.0 ng/g, limits of detection (LOD) of 0. 002, 0. 002, 0. 001 ng/g for α-HBCD, β-HBCD and γ-HBCD, respectively. The established method is therefore suitable for the determination of HBCDs and its diastereoisomers in fish feeds and fish samples at trace levels. Using the established method, HBCDs were detected in 4 of 25 fish feeds and in 3 of 30 fish samples. Positive rates of α-HBCD, β-HBCD and γ-HBCD in fish feed samples were all 16%; Positive rates of α-HBCD, β-HBCD and γ-HBCD in fish samples were 10%, 6. 67%, and 10%, respectively. Bioaccumulation factors (BMF), ratio of HBCDs content in fish samples to those in fish feeds, were 0. 78 for α-HBCD, 0. 45 for β-HBCD and 1. 08 for γ-HBCD. Moderate pearson correlation coefficients were obtained for HBCDs between fish feed samples and fish samples, which show that HBCDs may be transferred to fish through fish feeds.
关 键 词:六溴环十二烷 高效液相色谱-电喷雾串联质谱 同位素稀释 基质固相分散 生物累积因子
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