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Gas chromatographic analysis of alcohols in blood with a chemometric approach

机译:用化学计量学方法对血液中酒精进行气相色谱分析

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The objective of the present study is to examine the main and interactive effects of different factors related with headspace-solid phase extraction (HS-SPME) and gas chromatography (GC) conditions for the simultaneous determination of alcohols (ethanol, methanol, isopropanol, n-propanol) and acetone in blood samples. In order to evaluate the simultaneous effects of the significant variables, a chemometric approach was utilized to reveal the important parameters. The factors affecting the headspace extraction of alcohols on the SPME fiber was first deduced in a screening study by applying a Placketta€“Burman design. According to the screening results, the factors that possess a positive effect on peak areas are sample concentration, inlet temperature, flow rate for the carrier gas and volume of the solution. Based on the results of the screening study, to continue optimization, six insignificant values were fixed at the appropriate amounts (oven temperature: 50 ?°C; detector temperature: 250 ?°C; H2 gas flow rate: 35 mL mina?’1; split flow rate: 30 mL mina?’1; equilibrium temperature: 55 ?°C, extraction time: 4 min). Subsequently, a central composite design (CCD) was constructed for optimization and response surface methodology (RSM) was used to interpret the effect of each pair of independent variables on the response. The optimized method for alcohol and acetone analysis via HS-SPME-GC was validated through spike recovery tests.
机译:本研究的目的是研究与顶空固相萃取(HS-SPME)和气相色谱(GC)条件相关的不同因素的主要相互作用和相互作用,以便同时测定醇(乙醇,甲醇,异丙醇, -丙醇)和丙酮在血液样本中的含量。为了评估重要变量的同时作用,使用了化学计量学方法来揭示重要参数。在筛选研究中,首先采用Placketta-Burman设计推导了影响SPME纤维上醇顶空萃取的因素。根据筛选结果,对峰面积产生积极影响的因素是样品浓度,入口温度,载气流速和溶液体积。根据筛选研究的结果,为继续进行优化,将六个无关紧要的值固定在适当的量(烤箱温度:50°C;检测器温度:250°C;氢气流量:35 mL mina-1)。 ;分流流速:30mL min-1;平衡温度:55℃,萃取时间:4min。随后,构建了用于优化的中央复合设计(CCD),并使用响应面方法(RSM)来解释每对独立变量对响应的影响。通过加标回收测试验证了通过HS-SPME-GC进行乙醇和丙酮分析的优化方法。

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