用于同时测定（感冒-流感）糖浆剂型中对乙酰氨基酚、伪麻黄碱、氯苯那敏和苯甲酸钠四元混合物的稳定性指示新型反相超高效液相色谱法

Stability-Indicating New RP-UPLC Method for Simultaneous Determination of a Quaternary Mixture of Paracetamol, Pseudoephedrine, Chlorpheniramine, and Sodium Benzoate in (Cold-Flu) Syrup Dosage Form.

作者信息

Mohamed Mahmoud A

机构信息

Quality Control, Hikma Pharmaceutical Company, Beni-Suef, Egypt.

出版信息

J AOAC Int. 2022 Apr 27;105(3):703-716. doi: 10.1093/jaoacint/qsac002.

DOI:10.1093/jaoacint/qsac002

PMID:35015880

Abstract

BACKGROUND

A combination of paracetamol, pseudoephedrine, chlorpheniramine, and sodium benzoate in (Cold-Flu) 1,2,3 Syrup dosage form is specified for the treatment of common cold and flu symptoms.

OBJECTIVE

The functional role of this study is to develop a novel, reliable, and selective stability-indicating reversed-phase ultra-performance liquid chromatography (RP-UPLC) method for simultaneous identification of a quaternary mixture of paracetamol, pseudoephedrine, chlorpheniramine, and sodium benzoate in (Cold-Flu) 1,2,3 Syrup dosage form.

METHOD

The specific method is accomplished using an Acquity UPLC HSS T3 C18 column (2.1 mm × 100 mm), 1.8 µm particle size with pore size 100 Å, utilizing a mixture of purified water-methanol-trifluoroacetic acid (72.5:27.5:1.5, v/v) as the mobile phase at a flow rate of 0.3 mL/min. The column void volume is 1.15 min. UPLC detection is adjusted at 205 nm using a photodiode array detector.

RESULTS

Calibration curves are obtained in the linearity ranges: 25-500 µg/mL for paracetamol, 10-50 µg/mL for pseudoephedrine, 0.5-5 µg/mL for chlorpheniramine, and 3-30 µg/mL for sodium benzoate with a correlation coefficient > 0.9992. The mean recovery of the developed method is tested and shows good recovery results between 99-101%; selectivity and forced degradation studies are investigated as per the International Council for Harmonisation Guidelines and no interference is detected due to degradation peaks.

CONCLUSION

The proposed stability-indicating UPLC method for simultaneous determination of the three drugs, paracetamol, pseudoephedrine, and chlorpheniramine, with a preservative sodium benzoate in (Cold-Flu) 1,2,3 Syrup dosage form is successfully accomplished, developed, and validated, and can be easily used in the analysis of drugs in pure or dosage form.

HIGHLIGHTS

The novelty of the current research work lies in the development of the UPLC method for simultaneous determination of a quaternary mixture of paracetamol, pseudoephedrine, chlorpheniramine, and sodium benzoate in (Cold-Flu) 1,2,3 Syrup dosage form.

摘要

背景

（感冒流感）1、2、3糖浆剂型中的对乙酰氨基酚、伪麻黄碱、氯苯那敏和苯甲酸钠组合用于治疗普通感冒和流感症状。

目的

本研究的功能作用是开发一种新颖、可靠且具有选择性的稳定性指示反相超高效液相色谱（RP-UPLC）方法，用于同时鉴定（感冒流感）1、2、3糖浆剂型中对乙酰氨基酚、伪麻黄碱、氯苯那敏和苯甲酸钠的四元混合物。

方法

具体方法采用 Acquity UPLC HSS T3 C18 柱（2.1 mm×100 mm），粒径 1.8 µm，孔径 100 Å，以纯化水 - 甲醇 - 三氟乙酸（72.5:27.5:1.5，v/v）的混合物作为流动相，流速为 0.3 mL/min。柱空体积为 1.15 min。使用光电二极管阵列检测器在 205 nm 处进行 UPLC 检测。

结果

获得校准曲线的线性范围为：对乙酰氨基酚 25 - 500 µg/mL、伪麻黄碱 10 - 50 µg/mL、氯苯那敏 0.5 - 5 µg/mL、苯甲酸钠 3 - 30 µg/mL，相关系数 > 0.9992。对所开发方法的平均回收率进行测试，显示回收率良好，在 99 - 101%之间；按照国际协调理事会指南进行选择性和强制降解研究，未检测到降解峰产生干扰。