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Determination of trapidil in human serum and urine by derivative UV spectrophotometry after selective solid-phase extraction

机译:选择性固相萃取-导数紫外分光光度法测定人血清和尿液中的曲非定

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摘要

A novel analytical technique able to determine the anti-ischemic drug trapidil in human serum and urine is proposed. In order to achieve satisfactory sensitivity and selectivity, an extraction procedure was required to isolate the drug from complex matrixes such as serum and urine. A solid-phase extraction procedure was investigated to both increase the analyte concentration and eliminate the interfering molecules present in large amounts in both matrixes. Optimization of the extraction step was realized by selecting a new polymeric sorbent based on a surface-modified styrene–divinylbenzene polymer which provided fast and efficient drug extraction. Drug quantification was performed by using the third-order derivative spectra of the SPE eluates. Absorbance specific signals at 3D335,316 and 3D316 nm for urine and serum, respectively, were demonstrated to be directly proportional to drug concentration and barely affected by residual matrix interferences. Under the optimized experimental conditions the calibration plots were linear over the concentration range 0.2–50 μg mL?1. The method was validated by analysis of a series of spiked samples. Accuracy (recovery of 95 and 94% for serum and urine, respectively) and precision (RSD below 4%) were good.
机译:提出了一种能够测定人血清和尿液中抗缺血性药物特拉替尼的新颖分析技术。为了获得令人满意的灵敏度和选择性,需要采用提取程序从复杂的基质(例如血清和尿液)中分离药物。研究了固相萃取程序,以增加分析物的浓度并消除两种基质中大量存在的干扰分子。通过选择一种新的基于表面改性的苯乙烯-二乙烯基苯聚合物的聚合物吸附剂,可以实现萃取步骤的优化,该吸附剂可提供快速有效的药物萃取。通过使用SPE洗脱液的三阶导数光谱进行药物定量。尿液和血清分别在3 335、316 和3 316的吸光度信号与药物浓度成正比,几乎不受残留基质的影响干扰。在优化的实验条件下,校准曲线在0.2–50μgmL?1 的浓度范围内是线性的。通过分析一系列加标样品验证了该方法。准确性(血清和尿液回收率分别为95%和94%)和准确性(RSD低于4%)都不错。

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