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High-Performance Liquid Chromatographic Determination of Propofol in Human Plasma: Comparison of Different Heteroscedastic Calibration Curve Models

机译:高效液相色谱法测定人血浆中的异丙酚:不同的异方差校正曲线模型的比较

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Purpose: The aim of this study was to select the best calibration model for determination of propofol plasma concentration by high-performance liquid chromatography method. Methods: Determination of propofol in plasma after deproteinization with acetonitrile containing thymol (as internal standard) was carried out on a C18 column with a mixture of acetonitrile and trifluoroacetic acid 0.1% (60:40) as mobile phase which delivered at the flow rate of 1.2 mL/minute . Fluorescence detection was done at the excitation and emission wavelengths of 276 and 310 nm, respectively. After fitting different equations to the calibration data using weighted regression, the adequacy of models were assessed by lack-of-fit test, significance of all model parameters, adjusted coefficient of determination (R2adjusted) and by measuring the predictive performance with median relative prediction error and median absolute relative prediction error of the validation data set. Results: The best model was a linear equation without intercept with median relative prediction error and median absolute relative prediction error of 4.0 and 9.4%, respectively in the range of 10-5000 ng/mL. The method showed good accuracy and precision. Conclusion: The presented statistical framework could be used to choose the best model for heteroscedastic calibration data for analytes like propofol with wide range of expected concentration.
机译:目的:本研究的目的是选择最佳的校准模型,以通过高效液相色谱法测定丙泊酚血浆浓度。方法:在C18色谱柱上以乙腈和0.1%三氟乙酸(60:40)作为流动相的混合物,在流动相为的条件下,以含有百里香酚(内标)的乙腈脱蛋白后测定血浆中的异丙酚。 1.2 mL /分钟。分别在激发和发射波长276和310 nm处进行荧光检测。在使用加权回归将不同的方程式拟合到校准数据后,通过缺乏拟合检验,所有模型参数的重要性,调整后的确定系数(R2调整后)以及通过测量具有中位数相对预测误差的预测性能来评估模型的充分性以及验证数据集的绝对绝对中位数预测误差。结果:最佳模型是没有截距的线性方程,其中位数相对预测误差和中位数绝对相对预测误差分别在10-5000 ng / mL范围内,分别为4.0和9.4%。该方法显示了良好的准确性和准确性。结论:所提出的统计框架可用于为预期浓度范围较广的丙泊酚等分析物的异方差校准数据选择最佳模型。

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