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新型五溴苄基柱在高效液相色谱法同时测定八种抗真菌药物中的应用。

Novel Application of Pentabromobenzyl Column for Simultaneous Determination of Eight Antifungal Drugs Using High-performance Liquid Chromatography.

机构信息

Department of Analytical Chemistry, Faculty of Pharmacy Helwan University, Cairo 11795, Egypt.

Department of Pharmaceutical and Medicinal Chemistry, Pharmaceutical and Drug Industries Research Division, National Research Centre, Dokki 12622, Giza, Egypt.

出版信息

Comb Chem High Throughput Screen. 2020;23(10):991-1001. doi: 10.2174/1386207323666200220114818.

Abstract

AIM

A new, accurate and sensitive reversed-phase high-performance liquid chromatography (RP-HPLC) as an analytical method for the quantitative determination of eight antifungal drugs in spiked human plasma has been described optimized and validated.

MATERIALS AND METHODS

The analyzed compounds were voriconazole (VOR), luliconazole (LUL), clotrimazole (CLO), tioconazole (TIO), posaconazole (POS), ketoconazole (KET), sertaconazole (SER) and terconazole (TER).

RESULTS

The separation of the analyzed compounds was conducted using a novel pentabromobenzyl column known as COSMOSIL PBB-R (150 mm × 4.6 mm I.D., particle size 5 μm). The analysis of the studied drugs was determined within 14 min using a diode array detector and the mobile phase consisted of: 10 mM potassium dihydrogen phosphate buffer (pH 2.1): Methanol (2: 98 v/v). A linear response was observed for all compounds in the range of concentration studied. Sample preparation was done through liquid-liquid extraction using diethyl ether.

CONCLUSION

This proposed method was validated in terms of linearity, limit of quantification, limit of detection, accuracy, precision and selectivity. The method was successfully applied for the determination of these drugs in their pharmaceutical formulations and in human plasma samples.

摘要

目的

描述了一种新的、准确和灵敏的反相高效液相色谱(RP-HPLC)分析方法,用于定量测定人血浆中 8 种抗真菌药物。

材料与方法

分析的化合物为伏立康唑(VOR)、卢立康唑(LUL)、克霉唑(CLO)、噻康唑(TIO)、泊沙康唑(POS)、酮康唑(KET)、司他康唑(SER)和特康唑(TER)。

结果

使用一种新型的五溴苄基柱 COSMOSIL PBB-R(150mm×4.6mmID,粒径 5μm)进行了分析物的分离。使用二极管阵列检测器,在 14 分钟内完成了对研究药物的分析,流动相由 10mM 磷酸二氢钾缓冲液(pH2.1):甲醇(2:98v/v)组成。所有化合物在研究浓度范围内均表现出线性响应。样品制备通过使用二乙醚进行液-液萃取进行。

结论

该方法在线性、定量下限、检测限、准确度、精密度和选择性方面均得到了验证。该方法成功应用于这些药物在其制剂和人血浆样品中的测定。

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