首页> 外文期刊>Forensic science international >The GC/MS analysis of some commonly used non-steriodal anti-inflammatory drugs (NSAIDs) in pharmaceutical dosage forms and in urine.
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The GC/MS analysis of some commonly used non-steriodal anti-inflammatory drugs (NSAIDs) in pharmaceutical dosage forms and in urine.

机译:药物剂型和尿液中某些常用的非甾体类抗炎药(NSAID)的GC / MS分析。

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摘要

All the commonly used non-steriodal anti-inflammatory drugs (NSAIDs), except mefenamic acid, when extracted from the pharmaceutical dosage forms or the urines of users, and derivatized by silylation and then analysed by GC/MS, gave the mono- or the di-trimethylsilyl derivatives (depending on the number of derivatized groups in the drug) as the sole products. Mefenamic acid gave a mixture of products. When extracted from pharmaceutical dosage froms or from the urines of users, and analysed by GC/MS without derivatization, some of the NSAIDs were separated and detected as the unchanged molecules as the sole products, while others were separated and detected in altered forms as sole products or mixtures, depending on: (a) the solvent in which the extract was dissolved for injection into GC/MS, (b) the chemical structure of the drug, and (c) specifically for diflunisal, the presence or absence of potential methylating and/or acetylating agents on the GC column and/or septum. The main thermally-induced reactions of the underivatized NSAIDs included (i) methyl ester formation at the COOH group when the extract was dissolved in methanol, (ii) decarboxylation (i.e., loss of CO2), (iii) dehydration (i.e., loss of H2O) when the chemical structure permitted, such as for diclofenac, and (iv) cleavage at a carbon-heterocyclic nitrogen bond when one is present in an NSAID. Heating the urine in approximately 2 M HCl at 100 degrees C for 30 min, has been found to be a satisfactory means for effecting hydrolysis of the NSAIDs glucuronide conjugates. No metabolites, resulting from aromatic-ring hydroxylation, have been detected in urine for any of the NSAIDs studied.
机译:从苯甲酸中提取除甲芬那酸外,所有常用的非杀菌抗炎药(NSAID)均从使用者的剂型或使用者的尿液中提取,并通过甲硅烷基化进行衍生化,然后通过GC / MS分析,得出单或作为唯一产品​​的二三甲基甲硅烷基衍生物(取决于药物中衍生基团的数量)。甲芬那酸产生产物混合物。当从用户的剂量或使用者的尿液中提取药物,并通过GC / MS进行分析而不进行衍生化时,一些NSAID被分离出来并作为唯一的产物检测为未改变的分子,而其他NSAID则被分离出来并以改变的形式作为唯一的产物进行了检测。产物或混合物,取决于:(a)将提取物溶解在其中的溶剂以注入到GC / MS中;(b)药物的化学结构;(c)对于二氟菊酯,是否存在潜在的甲基化和/或GC柱和/或隔垫上的乙酰化剂。未衍生化的NSAID的主要热诱导反应包括(i)将提取物溶解在甲醇中时在COOH基上形成甲酯;(ii)脱羧(即CO2损失);(iii)脱水(即H2O损失)。 H2O)(如双氯芬酸)所允许的化学结构,以及(iv)NSAID中存在一个碳-杂环氮键时裂解。已经发现将尿液在约2 M HCl中于100摄氏度加热30分钟,是实现NSAIDs葡糖醛酸苷共轭物水解的令人满意的方法。对于所研究的任何NSAID,在尿液中均未检测到因芳香环羟基化而产生的代谢物。

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