Ebel S, Schütz H
Arzneimittelforschung. 1977 Feb;27(2):325-37.
The article describes analytical methods concerning screening tests for clonazepam and nitrazepam and the 7-amino derivatives. Further a detailed method is reported for the separation and identificatin of the benzodiazepine pair de. The method described permits a sharp separation and the nitro compounds with TiCl3 on the plate and forming the 7-acetamido derivatives by subsequent separation in the second dimension with ethyl acetate/acetic anhydride. The method described permits a sharp separation and highly sensitive detection by diazotization and coupling with Bratton-Marshall reagent. Amounts as low as 0.02 microng per spot can be detected. Besides preparation methods are reported for 7-aminoclonazepam, 7-acetaminoclonazepam, 2-amino-2'-chloro-5-nitrobenzophenone and 2,5-diamino-2'-chlorobenzophenone. Also spectral data (UV, IR, MS) and a literature review are given.
本文描述了有关氯硝西泮、硝西泮及其7-氨基衍生物筛查试验的分析方法。此外，还报告了一种用于分离和鉴定苯二氮䓬对的详细方法。所述方法能够实现清晰分离，通过在板上用TiCl3处理硝基化合物并在第二维中用乙酸乙酯/乙酸酐进行后续分离来形成7-乙酰氨基衍生物。所述方法能够实现清晰分离，并通过重氮化和与布拉顿-马歇尔试剂偶联进行高灵敏度检测。每点低至0.02微克的量都能被检测到。此外，还报告了7-氨基氯硝西泮、7-乙酰氨基氯硝西泮、2-氨基-2'-氯-5-硝基二苯甲酮和2,5-二氨基-2'-氯二苯甲酮的制备方法。同时还给出了光谱数据（紫外、红外、质谱）和文献综述。
