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针对两种二元混合物中莫匹罗星及其杂质测定所开发的两种色谱方法的绿色度评估

Greenness assessment of two chromatographic methods developed for the determination of Mupirocin in two binary mixtures along with its impurity.

作者信息

Galal Maha M, Abdullah Shaaban A, Mohamed Ola Y, Moustafa Azza A

机构信息

Analytical Chemistry Department, Faculty of Pharmacy, Cairo University, Kasr El-Aini street, Cairo, 11562, Egypt.

Egyptian Drug Authority-Central Administration for Drug Control (EDA-CADC), Cairo, Egypt.

出版信息

BMC Chem. 2023 Oct 27;17(1):145. doi: 10.1186/s13065-023-01055-5.

Abstract

Two simple, accurate and precise chromatographic methods have been developed and validated for estimating Mupirocin (MUP) in two binary mixtures. Mixture (1); with Fluticasone propionate (FLU) together with two of their impurities, namely; Pseudomonic acid-D (Pseud-D) and Fluticasone impurity C (FIC). Mixture (2); with Mometasone furoate (MF) along with Pseud-D impurity. High performance thin layer chromatography (HPTLC-densitometry) and high performance liquid chromatography (RP-HPLC) were the two proposed methods. In the HPTLC method, good separation of both mixtures was achieved by using HPTLC plates pre-coated with silica gel 60 F as stationary phase and the mobile phase consisted of toluene: chloroform: ethanol at a ratio of (5: 4: 2, by volume). The detection was carried out at 220 nm for MUP and 254 nm for FLU, MF, Pseud-D and FIC. In the HPLC method, chromatographic separation was carried out using Agilent Eclipse XDB (250 mm×4.6 mm, 5 μm) C18 column. For mixture (1), a mobile phase of methanol: sodium di-hydrogen phosphate (pH 3.0) was applied in stepwise gradient elution starting at ratios of (50: 50, v/v) and then switching to (80: 20, v/v) after 7 min at a flow rate of 1 mL.min. Detection was performed using diode array detector at 220 nm for MUP and Pseud-D and 240 nm for FLU and FIC. For mixture (2), the same mobile phase was used, but in isocratic elution in the ratio (80: 20, v/v) at flow rate of 1 mL.min and detection at 220 nm for MUP and Pseud-D and 248 nm for MF. The two methods successfully separated the cited drugs and were used to determine the drugs in pure form as well as pharmaceutical dosage forms. Validation was done as per International Council on Harmonization guidelines. Furthermore, the greenness of the proposed methods compared to the reported method, was evaluated as per the National Environmental Method Index, analytical Eco scale, Green Analytical Procedure Index and Analytical Greenness metric approaches.

摘要

已开发并验证了两种简单、准确且精密的色谱方法,用于测定两种二元混合物中的莫匹罗星(MUP)。混合物(1);含有丙酸氟替卡松(FLU)及其两种杂质,即假单胞菌酸-D(Pseud-D)和氟替卡松杂质C(FIC)。混合物(2);含有糠酸莫米松(MF)以及Pseud-D杂质。所提出的两种方法为高效薄层色谱法(HPTLC-密度测定法)和高效液相色谱法(RP-HPLC)。在HPTLC法中,使用预先涂覆硅胶60 F的HPTLC板作为固定相,以甲苯:氯仿:乙醇(体积比为5:4:2)作为流动相,实现了两种混合物的良好分离。对MUP的检测在220 nm波长下进行,对FLU、MF、Pseud-D和FIC的检测在254 nm波长下进行。在HPLC法中,使用安捷伦Eclipse XDB(250 mm×4.6 mm,5μm)C18柱进行色谱分离。对于混合物(1),采用甲醇:磷酸二氢钠(pH 3.0)的流动相进行梯度洗脱,起始比例为(50:50,v/v),7分钟后切换至(80:20,v/v),流速为1 mL.min。使用二极管阵列检测器进行检测,对MUP和Pseud-D在220 nm波长下检测,对FLU和FIC在240 nm波长下检测。对于混合物(2),使用相同的流动相,但采用等度洗脱,比例为(80:20,v/v),流速为1 mL.min,对MUP和Pseud-D在220 nm波长下检测,对MF在248 nm波长下检测。这两种方法成功分离了上述药物,并用于测定纯品形式以及药物剂型中的药物。按照国际协调理事会指南进行了验证。此外,根据国家环境方法指数、分析生态尺度、绿色分析程序指数和分析绿色度度量方法,对所提出的方法与已报道方法相比的绿色度进行了评估。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/eb90/10612294/c75c3632b5d3/13065_2023_1055_Fig1_HTML.jpg

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