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Quantitative analysis of acetone in blood via headspace gas chromatography/flame ionization detection.

机译:通过顶空气相色谱/火焰电离检测对血液中的丙酮进行​​定量分析。

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摘要

Scope and method of study. The purpose of this research project was to develop and validate a method for the quantitation of acetone in blood using Headspace Gas Chromatography with Flame Ionization Detection. The following items were included in the development: preparation of standards and positive controls, testing the necessity of using salts, establishment of a suitable internal standard concentration, determination of an appropriate sample size, limit of detection calculation, establishing the linear dynamic range, testing for carryover effects, method validation including case samples, and checking the stability of samples containing acetone.;Findings and conclusions. The blood-acetone quantitation method was successfully developed and validated. Standards and controls were accurate and precise and yielded linear results. The addition of salt to sample vials was deemed unnecessary. An internal standard concentration of 0.05% (v/v) n-propanol in water and a sample size of 0.25 mL were found to be suitable. The limit of detection was calculated to be 0.333 mg/dL while the limit of quantitation was calculated to be 0.816 mg/dL. However, quantitations were inaccurate below 1.0 mg/dL and blood-acetone concentrations above 250.0 mg/dL are not generally encountered. Therefore, an administrative linear dynamic range was set from 1.0 to 250.0 mg/dL. No carryover between samples occurred. Interday and interindividual variations were 6.93 and 0.77%, respectively. When checking the stability of samples containing acetone, time accounted for 97.7% variation while temperature only accounted for 0.22% variation.
机译:研究范围和方法。该研究项目的目的是开发和验证一种使用带有火焰电离检测的顶空气相色谱法定量血液中丙酮的方法。开发中包括以下项目:制备标准品和阳性对照品,测试使用盐的必要性,确定合适的内标浓度,确定合适的样品量,检测限,建立线性动态范围,测试对于残留效应,包括案例样品在内的方法验证,以及检查含丙酮样品的稳定性。;发现和结论。血液丙酮定量方法已成功开发并验证。标准品和对照品准确而精确,并得出线性结果。认为无需在样品瓶中添加盐。发现内部标准浓度为0.05%(v / v)的正丙醇水溶液和0.25 mL的样品量是合适的。计算的检出限为0.333 mg / dL,而定量的检出限为0.816 mg / dL。但是,低于1.0 mg / dL的定量不准确,并且通常不会遇到高于250.0 mg / dL的血丙酮浓度。因此,管理线性动态范围设置为1.0到250.0 mg / dL。样品之间没有残留。日间和个体间差异分别为6.93和0.77%。当检查含丙酮的样品的稳定性时,时间占97.7%的变化,而温度仅占0.22%的变化。

著录项

  • 作者

    Talbert, Susan Lynn.;

  • 作者单位

    Oklahoma State University.;

  • 授予单位 Oklahoma State University.;
  • 学科 Health Sciences Toxicology.;Chemistry Biochemistry.;Chemistry Analytical.
  • 学位 M.S.
  • 年度 2009
  • 页码 72 p.
  • 总页数 72
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类 毒物学(毒理学);化学;生物化学;
  • 关键词

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