固相萃取-气相色谱法测定螺旋藻中指示性 多氯联苯

Determination of indicator polychlorinated biphenyls in Spirulina by solid-phase extraction and gas chromatography

中文关键词:  气相色谱法  指示性多氯联苯  螺旋藻

英文关键词:gas chromatography  indicator polychlorinated biphenyls  Spirulina

中文摘要:

      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, 0.25 μm)石英毛细管柱, 采用程序升温分离, 流速为1.0 mL/min, 进样量为1.00 μL, 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10~50 μg/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、45 μg/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。

英文摘要:

      Objective To establish a method for the determination of trace polychlorinated biphenyls in Spirulina by gas chromatography, so as to investigate the residues of 7 kinds of indicator polychlorinated biphenyls (PCBs) in Spirulina. Methods After extracted with acetonitrile, the sample extract was purified by Florisil column. Under the chromatographic conditions, the analysis was carried out with a capillary column (DB-17, 30 m×0.25 mm, 0.25 μm) at a flow rate of 1.0 mL/min, and the sample volume was 1.00 μL. Monitoring with an electron-capture detector, all the target analytes were separated by temperature-programming of the column. Results Good linearities were obtained in the range of 10~50 μg/L for 7 kinds of indicator PCBs with the correlation coefficients greater than 0.999 by external method. The average recoveries at three spiked levels of 25, 35 and 45 μg/kg of the 7 kinds of indicator PCBs in Spirulina ranged from 90.8% to 112% with the RSDs of 0.526%~3.89%. Conclusions This established method is simple, rapid and accurate, and can be used for the routine analysis for the indicator PCBs in Spirulina.