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Thermal (In)stability of Atropine and Scopolamine in the GC-MS Inlet

机译:热(IN)与GC-MS入口中阿托品和汽油胺的稳定性

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摘要

The intoxication due to unintentional or intentional ingestion of plant material containing tropane alkaloids is quite frequent. GC-MS method is still widely used for the identification of these toxicologically important substances in human specimen. During general unknown analysis, high temperature of inlet, at least 270 °C, is commonly used for less volatile substances. Unfortunately, both tropanes are thermally unstable and could be overlooked due to their degradation. The temperature-related degradation of tropanes atropine and scopolamine was systematically studied in the inlet of a GC-MS instrument in the range 110–250 °C by increments of 20 °C, additionally also at 275 °C, and in different solvents. At inlet temperatures not higher than 250 °C, the degradation products were formed by elimination of water and cleavage of atropine’s ester bond. At higher temperatures, elimination of formaldehyde became predominant. These phenomena were less pronounced when ethyl acetate was used instead of methanol, while n-hexane proved unsuitable for several reasons. At an inlet temperature of 275 °C, tropanes were barely detectable. During systematic toxicological analysis, any tropanes’ degradation products should indicate the possible presence of atropine and/or scopolamine in the sample. It is not necessary to prepare thermally stable derivatives for confirmation. Instead, the inlet temperature can be decreased to 250 °C, which diminishes their degradation to a level where their detection and identification are possible. This was demonstrated in several case studies.
机译:由于无意或有意地摄取含有晶醇生物碱的植物材料而导致的中毒是非常频繁的。 GC-MS方法仍然广泛用于鉴定人类标本中这些毒理学上重要物质。在一般未知的分析期间,高温入口,至少270℃,通常用于较少的挥发性物质。不幸的是,仿菠菜都是热不稳定的,并且由于它们的降解而可能被忽视。在110〜250℃的GC-MS仪器的入口处,通过20℃的增量,在110℃的仪器的入口处,在275℃,不同的溶剂中,在110〜250℃的入口处进行了温度相关的劣化。在不高于250℃的入口温度下,通过消除阿托品的酯键的水和切割来形成降解产物。在较高的温度下,消除甲醛变得主要。当使用乙酸乙酯代替甲醇时,这些现象不太明显,而N-己烷证明是不合适的。在275°C的入口温度下,Tropanes几乎无法检测到。在系统毒理学分析期间,任何双层的降解产物都应该表明样品中可能存在阿托嘌呤和/或汽油。没有必要制备热稳定的衍生物进行确认。相反,入口温度可以降至250℃,这将其降低到其检测和识别的水平。这是在几个案例研究中证明的。

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