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,0.25μm）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 method for the determination of trace polychlorinated biphenyls in Spirulinaby gas chromatography, so as to investigate the residues of 7 kinds of indicator polychlorinated biphenyls （PCBs） inSpirulina.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, 0.25μm） at a flow rate of 1.0 mL/min, and the sample volume was 1.00μL. 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 10~50μg/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 45μg/kg of the 7 kinds of indicator PCBs inSpirulina 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 inSpirulina.
出处
《食品安全质量检测学报》
CAS
2016年第12期4913-4918,共6页
Journal of Food Safety and Quality
基金
云南省科技创新平台建设计划(公共科技服务项目)(2014DA001)~~
关键词
气相色谱法
指示性多氯联苯
螺旋藻
gas chromatography
indicator polychlorinated biphenyls
Spirulina
