色谱

色谱 ›› 2014, Vol. 32 ›› Issue (11): 1266-1270.DOI: 10.3724/SP.J.1123.2014.06010

• 研究论文 • 上一篇    下一篇

双重净化-气相色谱法测定植物油中指示性多氯联苯

丁立平1, 蔡春平2, 王丹红2   

  1. 1. 福清出入境检验检疫局技术中心, 福建 福清 350300;
    2. 福建出入境检验检疫局技术中心, 福建 福州 350001
  • 收稿日期:2014-06-06 修回日期:2014-07-19 出版日期:2014-11-08 发布日期:2014-10-31
  • 通讯作者: 丁立平,E-mail:43548624@qq.com.
  • 基金资助:

    国家质检总局科技项目(2013IK148);福建出入境检验检疫局科技项目(FK2012-16,FK2013-18,FK2013-19).

Determination of indicator polychlorinated biphenyls in vegetable oils by double clean-up-gas chromatography

DING Liping1, CAI Chunping2, WANG Danhong2   

  1. 1. Technology Center of Fuqing Entry-Exit Inspection and Quarantine Bureau, Fuqing 350300, China;
    2. Technology Center of Fujian Entry-Exit Inspection and Quarantine Bureau, Fuzhou 350001, China
  • Received:2014-06-06 Revised:2014-07-19 Online:2014-11-08 Published:2014-10-31

PDF

163

被引次数

13

摘要：

为了考察食用油中7种指示性多氯联苯(PCBs)的残留情况,建立了食用油中痕量多氯联苯测定的双重净化-气相色谱法。以乙腈提取样品,提取液浓缩至干后用正己烷溶解,经浓硫酸、硅胶分散固相萃取双重净化后进行气相色谱分析,外标法定量。优化的色谱条件为:HP-5石英毛细管柱(30 m×0.32 mm×0.25 μm)程序升温分离,流速0.8 mL/min,进样量1.00 μL,电子捕获检测器检测。结果表明:在优化的条件下,7种多氯联苯在10~500 μg/L范围内线性良好,相关系数大于0.999,不同基质中的检出限(S/N=3)范围为1.8~8.9 μg/kg,定量限(S/N=10)范围为5.9~29.8 μg/kg。在橄榄油、花生油和棕榈油空白样品中添加10、20、100 μg/kg 3个水平的7种多氯联苯,其加标回收率范围为71.0%~105.5%,相对标准偏差(RSD)范围为4.0%~11.3%。该方法具有操作简便、快速、准确的特点,可用于植物油中指示性多氯联苯残留量的日常检测。

关键词: 残留量, 多氯联苯, 气相色谱, 双重净化, 植物油

Abstract:

To investigate the residues of seven indicator polychlorinated biphenyls (PCBs) in vegetable oils, a method was established for the determination of trace PCBs in vegetable oils by double clean-up coupled with gas chromatography (GC). After extracted with acetonitrile, the sample extract was concentrated to dryness followed by re-dissolving with hexane. And the solution was pretreated by adding concentrated sulfuric acid followed cleaned-up with silica gel in dispersive solid-phase extraction protocol, then analyzed by GC with external standard method. Under the optimized chromatographic conditions, the analysis was carried out with a capillary column (HP-5, 30 m×0.32 mm×0.25 μm) at a flow rate of 0.8 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. Good linearities were obtained in the range of 10-500 μg/L for the seven indicator PCBs with the correlation coefficients greater than 0.999. For different matrices, the limits of detection (S/N=3) and limits of quantitation (S/N=10) were in the range of 1.8-8.9 μg/kg and 5.9-29.8 μg/kg, respectively. At three spiked levels of 10, 20 and 100 μg/kg of the seven indicator PCBs in olive oil, palm oil and peanut oil blank samples, the average recoveries ranged from 71.0% to 105.5% with the RSDs of 4.0%-11.3%. The method is simple, rapid and accurate, and can be used for the routine analysis of the indicator PCBs in vegetable oils.

Key words: double clean-up, gas chromatography (GC), polychlorinated biphenyls (PCBs), residues, vegetable oils

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