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测定卡托普利的高效液相色谱法:水凝胶膜渗透性试验的实证研究。

High-performance liquid chromatography method for measuring Captopril: an empirical study on hydrogel film permeability test.

作者信息

Fatriyah Siti, Nizardo Noverra Mardhatillah, Ramadon Delly

机构信息

Department of Chemistry, Faculty of Mathematics and Natural Sciences, Universitas Indonesia, Depok, Indonesia.

Faculty of Pharmacy, Universitas Indonesia, Depok, Indonesia.

出版信息

Daru. 2024 Dec 20;33(1):8. doi: 10.1007/s40199-024-00552-9.

Abstract

BACKGROUND

High-performance liquid chromatography (HPLC) has emerged as a highly sensitive and versatile analytical technique for quantifying antihypertensive drugs, such as Captopril (CAP). This study focused on the optimization and validation of an HPLC method for quantifying CAP in an in vitro hydrogel permeability test.

OBJECTIVES

The main objective of this study was to develop and validate an HPLC method for quantifying CAP in an in vitro hydrogel permeability test.

METHODS

The HPLC method employed a C18 column (Waters, Sunfire, 5 μm; 250 × 4.6 mm) and a mobile phase consisting of methanol-water (85% v/v orthophosphoric acid) in a 55:45 (v/v) ratio at a flow rate of 0.5 mL/min. The UV-Vis detector was configured to detect CAP at a wavelength of 220 nm. The hydrogel film used in the permeability test was prepared using poly (vinyl alcohol)/poly (vinyl caprolactam) (PVA/PNVCL) with citric acid as a crosslinking agent.

RESULTS

All results met the validation parameters according to ICH Guideline. The HPLC method showed consistent retention time (4.7-4.9 min), linearity (1-50 µg/mL; r = 0.9995), accuracy (98.11-101.78%), precision (RSD ≤ 2%), and LoD/LoQ (0.19/0.62 µg/mL). The developed HPLC method was successfully applied to an in vitro permeability test using horizontal diffusion cells. The results demonstrated that CAP permeated through the swollen hydrogel film, with a cumulative drug permeation exceeding 30%.

CONCLUSION

This highlighted the method's utility in assessing drug transport properties through hydrogels. The validated HPLC method demonstrates robustness and reliability for quantifying CAP in the hydrogel permeability test.

摘要

背景

高效液相色谱法(HPLC)已成为一种用于定量分析抗高血压药物(如卡托普利(CAP))的高灵敏度且通用的分析技术。本研究聚焦于优化和验证一种用于体外水凝胶渗透性试验中定量测定CAP的HPLC方法。

目的

本研究的主要目的是开发并验证一种用于体外水凝胶渗透性试验中定量测定CAP的HPLC方法。

方法

该HPLC方法采用C18柱(沃特世,Sunfire,5μm;250×4.6mm),流动相为甲醇 - 水(含85% v/v正磷酸),比例为55:45(v/v),流速为0.5 mL/min。紫外 - 可见检测器设置为在220nm波长处检测CAP。渗透性试验中使用的水凝胶膜是用聚(乙烯醇)/聚(乙烯基己内酰胺)(PVA/PNVCL)并以柠檬酸作为交联剂制备的。

结果

所有结果均符合国际协调会议(ICH)指南的验证参数。该HPLC方法显示出一致的保留时间(4.7 - 4.9分钟)、线性(1 - 50μg/mL;r = 0.9995)、准确度(98.11 - 101.78%)、精密度(相对标准偏差≤2%)以及检测限/定量限(0.19/0.62μg/mL)。所开发的HPLC方法成功应用于使用水平扩散池的体外渗透性试验。结果表明CAP透过溶胀的水凝胶膜,药物累积透过率超过30%。

结论

这突出了该方法在评估药物通过水凝胶的传输特性方面的实用性。经过验证的HPLC方法在水凝胶渗透性试验中定量测定CAP时显示出稳健性和可靠性。

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