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NSAIDs Determination in Human Serum by GC-MS

机译：GC-MS测定人血清中的NSAID

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Non-steroidal anti-inflammatory drugs (NSAIDs) are being widely consumed without medical prescription and are often the cause of intoxication, usually in young children. For this, there is a special need in their determination in routine toxicology analysis. As screening methods mainly focus on drugs of abuse (DOA) that are alkaline compounds in their majority, they are not optimized for acidic drugs, such as NSAIDs. Thus, more specific methods are needed for the detection and quantification of this class of drugs. In this study, the efficient extraction of NSAIDs from blood serum and their accurate determination is studied. Optimum pH extraction conditions were studied and thereafter different derivatization procedures for their detection. From the derivatization reagents used, N , O -Bis(trimethylsilyl)trifluoroacetamide (BSTFA) with 1% Trimethylchlorosilane (TMCS) was found to be the optimum choice for the majority of the examined NSAIDs; pH of 3.7 was selected as the most efficient for the extraction step. Herein the formation of the lactam of diclofenac was also thoroughly investigated. The developed Gas Chromatography-Mass Spectrometry (GC-MS) method had a run time of 15 min with the mass spectrometer operating in Electron Impact (EI) within the mass range of 40 to 500 amu. The method was linear with R 2 above 0.991 and limits of quantitation (LOQ) ranging from 6 to 414 ng/mL. The intra-day accuracy and precision were found between 1.03%–9.79% and 88%–110%, respectively, and the inter-day accuracy and precision were between 1.87%–10.79% and 91%–113%. The optimum protocol was successfully applied to real clinical samples, where intoxication of NSAIDs was suspected.
机译：非甾体类抗炎药（NSAIDs）在没有医学处方的情况下被广泛食用，并且通常是中毒的原因，通常在幼儿中。为此，在常规毒理学分析中特别需要确定它们。由于筛选方法主要针对大多数为碱性化合物的滥用药物（DOA），因此并未针对酸性药物（例如NSAID）进行优化。因此，需要更具体的方法来检测和定量此类药物。在这项研究中，研究了从血清中有效提取NSAIDs及其准确测定方法。研究了最佳pH提取条件，然后检测了不同的衍生化程序。从所用的衍生化试剂中，发现N，O-双（三甲基甲硅烷基）三氟乙酰胺（BSTFA）和1％三甲基氯硅烷（TMCS）是大多数所检查的NSAID的最佳选择; pH值3.7被选为最有效的萃取步骤。在此，还彻底研究了双氯芬酸内酰胺的形成。研发的气相色谱-质谱（GC-MS）方法的运行时间为15分钟，质谱仪在电子冲击（EI）中运行，质量范围为40至500 amu。该方法是线性的，R 2高于0.991，定量限（LOQ）为6至414 ng / mL。日内准确性和精确度分别介于1.03％–9.79％和88％–110％之间，日间准确性和精确度介于1.87％–10.79％和91％–113％之间。最佳方案已成功应用于怀疑有NSAIDs中毒的实际临床样品。

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