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采用毛细管气相色谱法测定谷物及谷物制品中的熏蒸剂。

Determination of fumigants in cereals and cereal products by capillary gas chromatography.

作者信息

Van Rillaer W G, Beernaert H, Dejonckheere W

机构信息

Institute of Hygiene and Epidemiology, Food Division, Brussels, Belgium.

出版信息

Z Lebensm Unters Forsch. 1988 Aug;187(2):97-101. doi: 10.1007/BF01042617.

Abstract

This study describes two methods for the quantitative determination of the residual fumigants ethylene dichloride (EDC), carbon tetrachloride (CCl4), trichloroethylene (TCE), ethylene dibromide (EDB) and tetrachloroethylene (PCE) in cereals (especially wheat) and other foodstuffs. In the first method, a micro steam distillation- solvent extraction apparatus is used, while the second method is based on a headspace technique. For the quantitative determination of carbon tetrachloride in cereals, the multiple headspace technique is not retained because it is too time-consuming. The analysis of the different fumigants is performed by electron-capture gas chromatography, using a fused silica capillary column, CP sil 8 CB. With the steam distillation-solvent extraction method, recoveries from 95.9% to 100.5% are obtained for the fumigants, added at two different levels. The standard deviation varies between 1.1% and 6%. Using the simple headspace technique, recoveries from 73.5% to 85.1% with a standard deviation of between 1.7% and 6.6% have been reached for the fumigants in cereals fortified at two different levels. The absolute detection limits for the five fumigants EDC, CCl4, TCE, EDB and PCE, in both methods, are 30, 0.25, 1.1, and 0.5 pg, respectively.

摘要

本研究描述了谷物(尤其是小麦)和其他食品中残留熏蒸剂二氯乙烷(EDC)、四氯化碳(CCl4)、三氯乙烯(TCE)、二溴乙烷(EDB)和四氯乙烯(PCE)的两种定量测定方法。第一种方法使用微型水蒸气蒸馏 - 溶剂萃取装置,而第二种方法基于顶空技术。对于谷物中四氯化碳的定量测定,不采用多次顶空技术,因为它太耗时。通过电子捕获气相色谱法,使用熔融石英毛细管柱CP sil 8 CB对不同的熏蒸剂进行分析。采用水蒸气蒸馏 - 溶剂萃取法,在两个不同添加水平下,熏蒸剂的回收率为95.9%至100.5%。标准偏差在1.1%至6%之间。使用简单顶空技术,在两个不同添加水平下强化的谷物中,熏蒸剂的回收率为73.5%至85.1%,标准偏差在1.7%至6.6%之间。两种方法中,五种熏蒸剂EDC、CCl4、TCE、EDB和PCE的绝对检测限分别为30、0.25、1.1和0.5 pg。

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