同位素稀释高分辨气相色谱-高分辨磁质谱法测定大闸蟹中二噁英及其类似物

Determination of dioxins and their analogues in hairy crabs by isotope dilution high resolution gas chromatography and high resolution mass spectrometry

中文关键词:  同位素稀释  高分辨气相色谱法  高分辨磁质谱法  大闸蟹  二噁英

英文关键词:isotope dilution  high resolution gas chromatography  high resolution mass spectrometry  hairy crabs  dioxins

中文摘要:

      目的 建立同位素稀释高分辨气相色谱-高分辨磁质谱法测定大闸蟹中二噁英类化合物及二噁英类多氯联苯(dioxin-like polychlorinated biphenyls, DL-PCBs)的分析方法。方法 样品经加速溶剂萃取(丙酮:正己烷:二氯甲烷=20:40:40, V:V:V)、酸化硅胶初步净化、全自动二噁英净化系统净化后, 分别收集多氯代二苯并二噁英类／多氯代二苯并呋喃(polychlorinated dibenzo-p-dioxins, dibenzofurans, PCDD/Fs)、二噁英类多氯联苯的净化液, 浓缩后上机分析。采用同位素稀释内标法定量。结果 白肉PCDD/Fs的检出限为0.016~0.106 ng/kg, DL-PCBs的检出限为0.036~0.252 ng/kg; 棕肉PCDD/Fs的检出限为0.052~0.158 ng/kg, DL-PCBs的检出限为0.138~0.596 ng/kg。大闸蟹白肉PCDD/Fs、DL-PCBs的平均回收率分别为62.0%~103.8%、76.7%~93.5%; 相对标准偏差分别为6.7%~25.7%、9.8%~22.6%; 大闸蟹棕肉PCDD/Fs、DL-PCBs的平均回收率分别为56.8%~84.8%、60.9%~90.9%; 相对标准偏差分别为8.4%~25.8%、12.6%~24.1%。结论 本研究建立的方法灵敏度高、干扰小, 能满足国内外的检测需要。

英文摘要:

      Objective To establish a method for the determination of dioxins and dioxin-like polychlorinated biphenyls (DL-PCBs) in hairy crabs by isotope dilution high resolution gas chromatography-high resolution magnetic mass spectrometry. Methods Samples were extracted with accelerated solvent (acetone:hexane:dichlo romethane=20:40:40, V:V:V), initially purified by acidified silica gel, and purified by automatic dioxin purification system. The purification of polychlorinated dibenzo-p-dioxins, dibenzofurans (PCDD/FS) and purification liquid of dioxin polychlorinated biphenyls were collected. After concentration, the purged liquor was analyzed on the machine. Isotope dilution internal standard method was used for quantification. Results The limits of detection of PCDD/FS in white meat were 0.016?0.106 ng/kg, and the limits of detection of DL-PCBs were 0.036?0.252 ng/kg. The limits of detection of PCDD/FS in brown meat were 0.052?0.158 ng/kg, and the limits of detection of DL-PCBs were 0.138?0.596ng/kg. The average recoveries of PCDD/FS and DL-PCBs in white meat of hairy crab were 62.0%?103.8% and 76.7%?93.5%, respectively. The relative standard deviations were 7.0%?25.7% and 9.8%?22.6%, respectively. The average recoveries of PCDD/FS and DL-PCBs in brown meat of hairy crab were 56.8%?84.8% and 60.9%?90.9%, respectively. The relative standard deviations were 8.4%?23.7% and 12.6%?24.1%, respectively. Conclusion The method established in this study has high sensitivity and low interference, and can meet the needs of detection at home and abroad.