食品科学 ›› 2016, Vol. 37 ›› Issue (24): 222-227.doi: 10.7506/spkx1002-6630-201624035

• 安全检测 • 上一篇    下一篇

双重净化-气相色谱法同时测定蛋及蛋制品中六六六、滴滴涕和指示性多氯联苯

许仁杰,蔡春平,丁立平,林佳庆,陈丽叶,方 婷,陈锦权   

  1. 1.福建农林大学食品科学学院,福建 福州 350001;2.福建出入境检验检疫局技术中心,福建 福州 350001; 3.福清出入境检验检疫局技术中心,福建 福清 350300
  • 出版日期:2016-12-25 发布日期:2016-12-21
  • 基金资助:
    国家质检总局科技项目(2015IK033);国家自然科学基金青年科学基金项目(31401597);福建出入境检验检疫局科技项目(FK2013-19);福建省科技计划项目(2016Y0085);福建省高水平大学建设项目(612014043);2015年中青年教师教育科研项目杰出人才计划项目

Simultaneous Determination of Hexachlorocyclohexanes, Dichlorodiphenyltrichloroethanes and Indicator Polychlorinated Biphenyls in Eggs and Egg Products by Double Depuration-Gas Chromatography

XU Renjie, CAI Chunping, DING Liping, LIN Jiaqing, CHEN Liye, FANG Ting, CHEN Jinquan   

  1. 1. College of Food Science, Fujian Agriculture and Forestry University, Fuzhou 350001, China; 2. Fujian Entry-Exit Inspection and Quarantine Bureau Technology Center, Fuzhou 350001, China; 3. Fuqing Entry-Exit Inspection and Quarantine Bureau Technology Center, Fuqing 350300, China
  • Online:2016-12-25 Published:2016-12-21

摘要: 建立同时测定蛋及蛋制品中六六六、滴滴涕和指示性多氯联苯残留量的双重净化-气相色谱法。样品经乙腈提取,浓硫酸和焙烧型水滑石双重净化后采用气相色谱分析和外标法定量。结果表明:与传统的磺化法相比,采用浓硫酸和焙烧型水滑石双重净化的效果更好,干扰物质少,且目标物提取更充分。在10~200 μg/L的添加水平内4 种六六六、2 种滴滴涕和7 种指示性多氯联苯的线性关系良好,相关系数均大于0.999。方法的检出限(RSN=3)范围为1.12~3.89 μg/kg,定量限(RSN=10)范围为3.73~12.97 μg/kg。添加10、20、100 μg/kg 3 个水平的4 种六六六、2 种滴滴涕和7 种指示性多氯联苯于鸡蛋液、咸蛋及皮蛋空白样品中,加标回收率范围为78.04%~105.05%,相对标准偏差范围为1.28%~7.55%。该方法操作简便快速、准确、灵敏,适用于蛋及蛋制品中六六六、滴滴涕和指示性多氯联苯残留量的快速测定。

关键词: 蛋, 蛋制品, 六六六, 滴滴涕, 指示性多氯联苯, 气相色谱法

Abstract: A double depuration-gas chromatography (DDGC) method was developed for the simultaneous determination of residues of hexachlorocyclohexanes (BHCs), dichlorodiphenyltrichloroethanes (DDTs) and indicator polychlorinated biphenyls (PCBs) in eggs and egg products. Samples were extracted with acetonitrile followed by double purification with concentrated sulfuric acid and calcined hydrotalcite. Then the analytes were analyzed by GC and quantified with an external standard method. Results showed that compared with the traditional sulfonation method, more thorough extraction and higher purification efficiency of the target analytes with less interferences were achieved by double-purification with concentrated sulfuric acid and calcined hydrotalcite. Good linearities were obtained for four BHCs, two DDTs, and seven PCBs with correlation coefficients greater than 0.999 in the range of 10–200 μg/L. The limits of detection (LODs) (RSN = 3) and limits of quantitation (LOQs) (RSN =10) of the GC method were 1.12–3.89 and 3.73–12.97 μg/kg, respectively. The recoveries of these analytes from liquid egg, preserved eggs and salted eggs ranged from 78.04% to 105.05%, with relative standard deviation (RSD) ranging from 1.28% to 7.55% at three spiked levels of 10, 20, and 100 μg/kg. The method was simple, rapid, accurate and sensitive, and it was suitable for rapid detection of PCBs, BHCs and DDTs residues in eggs and egg products.

Key words: eggs, egg products, hexachlorocyclohexanes (BHCs), dichlorodiphenyltrichloroethanes (DDTs), indicator polychlorinated biphenyls (PCBs), gas chromatography (GC)

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