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Determination of triflusal in human plasma by high performance liquid chromatography with automated column switching system

机译:高效液相色谱-自动柱切换系统测定人血浆中的三氟甲磺酸

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摘要

An analytical method of triflusal in human plasma was devel- oped using semi-microbore HPLC equipped with automated col- umn switching system. p- Toluic acid which is the structural ana- logue of triflusal, was used as an internal standard and 2 M HCI was employed as a stabilizer. The load phase and mobile phase were prepared using acetonitrile and 20 mM KH2PO4 with the vol- ume ratios of 10:90 (pH 2.5) and 43:57 (pH 2.3), respectively. The signals were monitored by a UV detector at 275 nm with flow-rate of load phase, 500 lJ.L/min, and mobile phase, 100 lJ.L/min, respectively. The retention time of triflusal and p-toluic acid was about 20.2 min and 16.4 min, respectively. The detec- tion limit. of triflusal in human plasma was 0.01 lJ.g/mL and the 1imit of quantitative analysis was 0.05 lJ.g/mL. The accuracy of the assay was from 97.76% to 116.51% while the intra-day and inter-day coeft'icient of variation of the same concentration range was less than 15%. This analytical method demonstrated excel- lent sensitivity, reproducibility, specificity, and speed using the plasma sample. This method could be successfully applied to evaluate the bioavailability of triflusal in human subjects without time-consuming sample clean-up after oral administration of low dose.
机译:使用配备自动色谱柱切换系统的半微孔HPLC开发了一种在人血浆中的三氟甲磺酸的分析方法。对甲酚的结构类似物对甲苯甲酸用作内标,2 M HCl用作稳定剂。用乙腈和20 mM KH2PO4分别以10:90(pH 2.5)和43:57(pH 2.3)的体积比制备负载相和流动相。信号由UV检测器在275 nm处进行监测,负载相的流速分别为500 lJ.L / min和流动相的流速为100 lJ.L / min。三氟甲磺酸和对甲苯甲酸的保留时间分别为约20.2分钟和16.4分钟。检测极限。人血浆中三氟尿嘧啶的含量为0.01 lJ.g / mL,定量分析的1个模拟值为0.05 lJ.g / mL。该测定的准确性为97.76%至116.51%,而同一浓度范围内的日内和日间变异系数小于15%。这种分析方法使用血浆样品显示出出色的灵敏度,重现性,特异性和速度。该方法可以成功地用于评估人类受试者中三氟甲磺酸的生物利用度,而无需在口服小剂量口服后进行费时的样品清理。

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