Simultaneous Uplc Assay for Oxitropium Bromide and Formoterol Fumarate Dihydrate in Pressurised Metered Dose Inhaler Products for Chronic Obstructive Pulmonary Disease

IF 1.7 4区 农林科学 Q3 CHEMISTRY, ANALYTICAL Journal of AOAC International Pub Date : 2023-12-18 DOI:10.1093/jaoacint/qsad134
Serdar Seckin, Serap Saglik Aslan
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Abstract

Backround Oxitropium Bromide (OB) and Formoterol Fumarate Dihydrate (FFD) are inhaler molecules that are widely used in the treatment of chronic lung diseases. Objective The goal of this work was to create a reversed phase-ultra performance liquid chromatography (RP-UPLC) technique for assay and identification of OB and FFD, as well as identification and estimate of its associated compounds in pressurised metered dose inhaler product (pMDI). Method Separation of oxitropium and formoterol peaks were enhanced on C18 (50 x 2.1 mm x 1.7 μm), UPLC column with Ethylene-Bridged-Hybrid technology, The mobile phase consists of buffer (0.07 M KH2PO4) and acetonitrile (80:20 v/v). The detector wavelength of 210 nm, flow rate of pump 0.6 mL/min and oven temperature for column were set at 25◦C. The injection volume was 10 μL. The method run time is 2 min. The mobile phase was used as the solvent. Results Retention times were 0.5 min. for OB and 1.0 min. for FFD. The assay analysis was lineear range for all analytes within the range for concentrations 0.03—14.8 µg/mL of OB, 0.01– 0.88 µg/mL of FFD. LOD values and LOQ values 0.009 µg/mL and 0.026 µg/mL for OB, 0.003 µg/mL and 0.009 µg/mL for FFD, respectively. Recoveries were obtained at 96.3% for OB and 97.2% for FFD. Precisions values were (as RSD%) ≤1.5%. Conclusions With the UPLC method developed and validated according to the current ICH guidelines, it is possible to simultaneously detect OB and FFD of assay analysis in pMDI products accurately, precisely and selectively, independent of the matrix effect. Highlights The present method is the first method in the literature based on the UPLC method for this purpose. The UPLC method is a time-saving method, it provides a faster and cheaper technique than the HPLC method.
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用于慢性阻塞性肺病的加压定量吸入器产品中溴化奥昔托铵和富马酸福莫特罗二水合物的 Uplc 同时测定
背景 溴化奥昔托品(OB)和富马酸福莫特罗二水合物(FFD)是广泛用于治疗慢性肺部疾病的吸入剂分子。这项工作的目的是创建一种反相超高效液相色谱(RP-UPLC)技术,用于测定和鉴定 OB 和 FFD,以及鉴定和估计加压计量吸入器产品(pMDI)中的相关化合物。采用乙烯-桥接-杂化技术的 C18 (50 x 2.1 mm x 1.7 μm)超高效液相色谱柱,流动相为缓冲液(0.07 M KH2PO4)和乙腈(80:20 v/v)。检测器波长为 210 nm,泵流速为 0.6 mL/min,色谱柱烘箱温度为 25◦C。进样量为 10 μL。方法运行时间为 2 分钟。以流动相为溶剂。结果 OB 的保留时间为 0.5 分钟,FFD 的保留时间为 1.0 分钟。在 OB 浓度为 0.03-14.8 µg/mL 和 FFD 浓度为 0.01- 0.88 µg/mL 的范围内,所有分析物的检测分析均在线性范围内。OB 和 FFD 的检出限和定量限分别为 0.009 微克/毫升和 0.026 微克/毫升,0.003 微克/毫升和 0.009 微克/毫升。OB 和 FFD 的回收率分别为 96.3% 和 97.2%。精确度值(RSD%)≤1.5%。结论 根据现行的 ICH 指南开发和验证的 UPLC 方法可以准确、精确和选择性地同时检测 pMDI 产品中的 OB 和 FFD。亮点 本方法是文献中第一种基于 UPLC 法的检测方法。超高效液相色谱法是一种省时的方法,与高效液相色谱法相比,它提供了一种更快、更便宜的技术。
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来源期刊
Journal of AOAC International
Journal of AOAC International 医学-分析化学
CiteScore
3.10
自引率
12.50%
发文量
144
审稿时长
2.7 months
期刊介绍: The Journal of AOAC INTERNATIONAL publishes the latest in basic and applied research in analytical sciences related to foods, drugs, agriculture, the environment, and more. The Journal is the method researchers'' forum for exchanging information and keeping informed of new technology and techniques pertinent to regulatory agencies and regulated industries.
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