QuEChERS-气相色谱法测定8种鱼肉中多氯联苯
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摘要
采用重量法,以脂肪含量不同的8种鱼为研究对象,考察了冷冻法和吸附法两种脱脂方式的适用性,并提出共萃物去除策略,即当共萃物含量大于6. 0 mg/mL时,-18℃下冷冻2 h结合加入150 mg/mL乙二胺-N-丙基硅烷和C18(重量比1:1)吸附剂可达到好的去除效果;而当共萃物含量为4. 5～6. 0 mg/mL、小于4. 5 mg/mL时,只需分别加入150 mg/mL和100 mg/mL吸附剂。考察了冷冻时间和吸附剂加入量对加标鱼肉样品中多氯联苯的气相色谱图峰形和峰面积的影响。结果表明,以该策略为基础的QuEChERS-气相色谱法适用于鱼肉样品中多氯联苯残留分析。
In this study,eight types of fish with different fat contents were selected to investigate the applicability of two fat removal methods( freezing and adsorption) by gravimetric method. Further,the removal strategy of co-extracts was proposed. When the co-extract content was more than 6. 0 mg/m L,the co-extract could be efficiently removed through freezing for 2 h at-18 ℃ combined with adding150 mg/m L of PSA and C18 adsorbents( w/w 1: 1). While when the co-extract content was ranged from 4. 5 to 6. 0 mg/m L or less than 4. 5 mg/m L,the sample purification employed only the adsorption by adding 150 mg/m L or 100 mg/m L adsorbents,respectively. In order to verify the reliability of this strategy,the effect of freezing time and the dosage of adsorbent on the chromatograms and signal responses of polychlorinated biphenyls( PCBs) spiked in fish samples was also investigated. The results showed that the QuEChERS-gas chromatography method based on the proposed strategy had good linearity,recovery,limit of quantification and precision,and was suitable for the analysis of PCBs residues in fish species.
In this study,eight types of fish with different fat contents were selected to investigate the applicability of two fat removal methods( freezing and adsorption) by gravimetric method. Further,the removal strategy of co-extracts was proposed. When the co-extract content was more than 6. 0 mg/m L,the co-extract could be efficiently removed through freezing for 2 h at-18 ℃ combined with adding150 mg/m L of PSA and C18 adsorbents( w/w 1: 1). While when the co-extract content was ranged from 4. 5 to 6. 0 mg/m L or less than 4. 5 mg/m L,the sample purification employed only the adsorption by adding 150 mg/m L or 100 mg/m L adsorbents,respectively. In order to verify the reliability of this strategy,the effect of freezing time and the dosage of adsorbent on the chromatograms and signal responses of polychlorinated biphenyls( PCBs) spiked in fish samples was also investigated. The results showed that the QuEChERS-gas chromatography method based on the proposed strategy had good linearity,recovery,limit of quantification and precision,and was suitable for the analysis of PCBs residues in fish species.
引文
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