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[食品、土壤和饮用水中多环芳烃的鉴定和测定方法]

[Method for identifying and determining polycyclic aromatic hydrocarbons in foods, soil and drinking water].

作者信息

Fritz W

出版信息

Nahrung. 1979;23(1):63-81. doi: 10.1002/food.19790230110.

Abstract

A method is described for identifying and determining polycyclic aromatic hydrocarbons in foods, soil and drinking water that, owing to the combination of extractive, chromatographic and spectrophotometric techniques, permits to detect 0,01 microgram of bezo(a)pyrene/kg in the presence of other polycyclic aromatic hydrocarbons. The preparation, pretreatment and concentration of the samples depend upon their nature. The isolation and separation of the polycyclic aromatic hydrocarbons are achieved with the aid of two consecutive thin-layer chromatographic systems, silica gel and acetylated cellulose. The subsequent identification and determination are based on the ulta-violet spectra (limit of detection, almost 0,5 microgram/ml) and, in the nanogram range, on the in situ fluorescence spectral analysis (limit of detection, 0,005 microgram of benzo(a)pyrene/spot). Fluorescence excitation and emission spectra obtained directly from the acetylated cellulose plate permit not only the reliable identification but also the determination of the polycyclic aromatic hycrocarbons; fluorescence transfer loci obtained under various conditions, the simultaneous determination. Depending upon the kinds of sample material, the recovery values range from 75 to 99.6% with a variation coefficient between 10.3 and 22.1%. Furthermore, a limiting value method is presented that permits to take yes-no decisions, by means of thin-layer chromatographic screening without using complicated measuring techniques, indicating whether or not the respective sample complies with the benzo(a)pyrene standard.

摘要

本文描述了一种用于鉴定和测定食品、土壤及饮用水中多环芳烃的方法。该方法结合了萃取、色谱和分光光度技术,能够在存在其他多环芳烃的情况下,检测出0.01微克/千克的苯并(a)芘。样品的制备、预处理和浓缩取决于其性质。借助硅胶和乙酰化纤维素这两种连续的薄层色谱系统实现多环芳烃的分离。后续的鉴定和测定基于紫外光谱(检测限约为0.5微克/毫升),在纳克范围内则基于原位荧光光谱分析(检测限为0.005微克苯并(a)芘/斑点)。直接从乙酰化纤维素板获得的荧光激发和发射光谱不仅能够可靠地鉴定多环芳烃,还能对其进行测定;在不同条件下获得的荧光转移位点可用于同时测定。根据样品材料的种类,回收率在75%至99.6%之间,变异系数在10.3%至22.1%之间。此外,还提出了一种极限值方法,通过薄层色谱筛选,无需使用复杂的测量技术即可做出是或否的判断,表明相应样品是否符合苯并(a)芘标准。

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