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目的建立气相色谱法测定螺旋藻中痕量多氯联苯的分析方法,以考查螺旋藻中7种指示性多氯联苯(polychlorinated biphenyls,PCBs)的残留情况。方法乙腈提取样品后,选用弗罗里矽柱对螺旋藻中指示性多氯联苯净化。色谱条件为:DB-17(30 m×0.25 mm,0.25μm)石英毛细管柱,采用程序升温分离,流速为1.0m L/min,进样量为1.00μL,电子捕获检测器检测。结果在优化的条件下,7种指示性多氯联苯在10~50μg/L范围内线性良好,相关系数(r)大于0.999,在螺旋藻空白样品中添加25、35、45μg/kg 3个水平的7种指示性多氯联苯,其加标回收率范围为90.8%~112%,相对标准偏差(RSD)范围为0.526%~3.89%。结论该方法具有操作简便、快速、准确的特点,适用于螺旋藻试样中指示性多氯联苯痕量残留的分析。
OBJECTIVE To establish a gas chromatographic method for the determination of trace PCBs in Spirulina platensis, in order to investigate the residues of seven kinds of indicative polychlorinated biphenyls (PCBs) in Spirulina platensis. Methods After the samples were extracted by acetonitrile, Fluoro-silica column was used to purify the indicated PCBs in Spirulina. The chromatographic conditions were as follows: DB-17 (30 m × 0.25 mm, 0.25 μm) quartz capillary column was programmed temperature-programmed separation, the flow rate was 1.0 m L / min, the injection volume was 1.00 μL, and electron capture detector detected. Results Under the optimized conditions, the linearity of 7 kinds of indicator polychlorinated biphenyls in the range of 10 ~ 50μg / L was good and the correlation coefficient (r) was greater than 0.999. Three spiked samples of 25, 35 and 45μg / kg The average recoveries ranged from 90.8% to 112% with relative standard deviations (RSDs) ranging from 0.526% to 3.89%. Conclusion The method is simple, rapid and accurate. It is suitable for the analysis of trace PCBs residues in spirulina samples.