Schleibinger H, Leberl C, Rüden H
Fachgebiet Hygiene der Technischen Universität Berlin.
Zentralbl Bakteriol Mikrobiol Hyg B Umwelthyg Krankenhaushyg Arbeitshyg Prav Med. 1988 Nov;187(1):44-55.
A procedure to determine nitrated polycyclic aromatic hydrocarbons from suspended particulate matter was developed. Depending on the organic amount needed, different prefractionation steps are described, starting from thin layer chromatography and solid phase extraction by a cartouche system for small amounts, reaching over column chromatography to preparative HPLC for extracts corresponding up to 1000m3. Prior to analysis Nitro-PAH were reduced to the corresponding amines by a modified method given by Jäger. After reduction these amines could be trapped selectively by ion change chromatography and eluted as a pure fraction with a mixture of methanol/isopropylamine 1/1. This mixture can be easily evaporated and the sample is redissolved in acetonitrile/water 80/20, buffered at pH 7.2 by 0.1 M Tris-buffer. 20 microliter of that solution is injected in a HPLC system with a reversed phase column (250 x 4 mm, 5 micron) and fluorescence detection. According to the strong fluorescence properties of amino-PAH detection limits of 5-50 pg could be achieved. Thus, depending on the preconcentration factor (up to 100 m3 per 200 microliter) these compounds could be detected in the range from 0.5-5 pg/m3.
开发了一种从悬浮颗粒物中测定硝化多环芳烃的方法。根据所需的有机物量,描述了不同的预分离步骤,从薄层色谱法和针对少量样品的卡套系统固相萃取开始,到柱色谱法,再到适用于相当于1000立方米提取物的制备型高效液相色谱法。在分析之前,通过耶格尔给出的改良方法将硝基多环芳烃还原为相应的胺。还原后,这些胺可以通过离子交换色谱法选择性捕获,并用甲醇/异丙胺1/1的混合物作为纯馏分洗脱。该混合物可以很容易地蒸发,样品重新溶解在乙腈/水80/20中,并用0.1M Tris缓冲液在pH 7.2下缓冲。将20微升该溶液注入具有反相柱(250×4毫米,5微米)和荧光检测的高效液相色谱系统中。根据氨基多环芳烃的强荧光特性,可实现5-50皮克的检测限。因此,根据预浓缩因子(每200微升高达100立方米),这些化合物的检测范围为0.5-5皮克/立方米。