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Method Development for the Detection of Basic/Weak Basic Drugs in Hair by LCMSMS: Comparison between Methanolic and Alkaline Extraction on Real Samples

机译:LCMSMS检测头发中基本/弱碱性药物的方法开发:真实样品中甲醇和碱性提取物的比较

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Detection of drugs in hair has become popular in recent years. The significantly long drug detection window (months) in hair has allowed the retrospective investigation and measurement of past consumption of drug. As the majority of drugs are basic, an extraction method was developed based on a methanolic solution for detection of basic/weak basic drugs in hair. It was compared with alkaline digestion (NaOH) followed by LLE. A filtration step with filtration vials was added and their materials were compared. After filtration, extracts were injected directly onto a C18 column coupled to Sciex ABI 2000 MSMS. The mobile phase was 50% methanol, 0.1% formic acid and 2 mM ammonium acetate (isocratic). Both methods were compared by applying them to real samples. Results showed that calibration was linear with r2 of 0.991-0.999 for 20 tested analytes. The matrix effect was assessed to be between 91.4%- 110.2% for 18 analytes. PTFE filter material showed better recoveries over the GMF and PVDF based filters. Stability of analytes during extraction in general was better with methanolic incubation rather than alkaline digestion. With regard to real sample recovery, 6 out of 10 analytes recovered better with alkaline digestion. In conclusion, the methanolic method is capable of extracting most basic drugs in hair samples but only part of the total incorporated drug. Therefore, these results suggest that a combination of both methods (methanolic and alkaline extractions) in hair sample processing for general detection of basic and weak basic drugs may produce better results. However, not all basic drugs are stable under alkaline digestion.
机译:近年来,头发中药物的检测变得很流行。头发中很长的药物检测窗口(数月)使我们可以回顾性调查和测量过去的药物消费情况。由于大多数药物是碱性药物,因此开发了一种基于甲醇溶液的提取方法,用于检测头发中的碱性/弱碱性药物。将其与碱消解(NaOH)和随后的LLE相比较。添加带有过滤瓶的过滤步骤,并比较其材料。过滤后,将提取物直接注射到与Sciex ABI 2000 MSMS偶联的C18色谱柱上。流动相为50%的甲醇,0.1%的甲酸和2 mM醋酸铵(等度)。通过将它们应用于真实样本进行比较。结果表明,对于20种被测分析物,校准与r2为0.991-0.999呈线性关系。对于18种分析物,基质效应估计在91.4%至110.2%之间。 PTFE过滤器材料比基于GMF和PVDF的过滤器具有更好的回收率。一般而言,甲醇孵育比碱性消化在分析过程中,分析物的稳定性更好。关于实际样品的回收率,十分之六的分析物通过碱消解可以更好地回收。总之,甲醇法能够提取头发样品中的大多数碱性药物,但仅能提取总掺入药物的一部分。因此,这些结果表明,在头发样品处理中对碱性和弱碱性药物进行常规检测的两种方法(甲醇提取和碱提取)的组合可能会产生更好的结果。但是,并非所有碱性药物在碱性消化下都是稳定的。

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