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HILIC-UV 技术在原料药和眼用凝胶中莫西沙星和氟康唑测定中的应用。

Implementation of HILIC-UV technique for the determination of moxifloxacin and fluconazole in raw materials and pharmaceutical eye gel.

机构信息

Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Mansoura University, Mansoura, 35516, Egypt.

出版信息

Sci Rep. 2022 Aug 4;12(1):13388. doi: 10.1038/s41598-022-17064-8.

DOI:10.1038/s41598-022-17064-8
PMID:35927412
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC9352657/
Abstract

Hydrophilic interaction liquid chromatography (HILIC) has inherent merits over RP-HPLC in the analyzing of hydrophilic substances. Accordingly, an innovative HILIC-UV methodology is proposed for the simultaneous estimation of ethyl paraben (PRN), fluconazole (FLZ) and moxifloxacin hydrochloride (MOX) in raw materials and pharmaceutical eye gel. The separation process was conducted using Waters XBridge™ HILIC column (100 mm × 4.6 mm, 3.5 μm particle size) at room temperature. Isocratic mobile phase containing acetonitrile: 0.1% triethylamine buffer (90:10, v/v, pH 5.0), was pumped at flow rate 1.0 mL/min and detected at 260 nm. Under these optimized conditions, PRN, FLZ and MOX showed rectilinear relationships with the concentration ranges (0.5-6.0), (5.0-50.0) and (5.0-60.0) μg/mL, respectively. The developed method offered at least fivefold increase in sensitivity within shorter time than the reported methods. Three greenness assessment tools namely: Analytical eco-scale, GAPI and AGREE were exploited to investigate the method's impact on the environment and conduct a comparative study with the reported methods. International council of Harmonization (ICH) guidelines have been followed to calculate validation parameters. The statistical comparison between results of the suggested method and the comparison method showed no discrepancy confirming accuracy of the method.

摘要

亲水作用色谱(HILIC)在分析亲水物质方面具有相对于反相高效液相色谱(RP-HPLC)的固有优势。因此,提出了一种创新的 HILIC-UV 方法,用于同时测定原料药和药用滴眼凝胶中对羟基苯甲酸乙酯(PRN)、氟康唑(FLZ)和盐酸莫西沙星(MOX)的含量。分离过程在 Waters XBridge™ HILIC 柱(100mm×4.6mm,3.5μm 粒径)上在室温下进行。等度流动相由乙腈:0.1%三乙胺缓冲液(90:10,v/v,pH5.0)组成,以 1.0mL/min 的流速泵入,并在 260nm 处检测。在这些优化的条件下,PRN、FLZ 和 MOX 的浓度范围分别为(0.5-6.0)、(5.0-50.0)和(5.0-60.0)μg/mL 时,均呈现出线性关系。与已报道的方法相比,该方法在更短的时间内提供了至少五倍的灵敏度提高。利用三种绿色评估工具,即:分析生态标度、GAPI 和 AGREE,来研究该方法对环境的影响,并与已报道的方法进行比较研究。已遵循国际协调会议(ICH)指南来计算验证参数。建议方法的结果与比较方法的统计比较没有差异,证实了该方法的准确性。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce7f/9352657/c8aa41adfa01/41598_2022_17064_Fig4_HTML.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce7f/9352657/158405151df7/41598_2022_17064_Fig1_HTML.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce7f/9352657/d7b9f231e15c/41598_2022_17064_Fig2_HTML.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce7f/9352657/7cd924e63109/41598_2022_17064_Fig3_HTML.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce7f/9352657/c8aa41adfa01/41598_2022_17064_Fig4_HTML.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce7f/9352657/158405151df7/41598_2022_17064_Fig1_HTML.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce7f/9352657/d7b9f231e15c/41598_2022_17064_Fig2_HTML.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce7f/9352657/7cd924e63109/41598_2022_17064_Fig3_HTML.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce7f/9352657/c8aa41adfa01/41598_2022_17064_Fig4_HTML.jpg

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