Saad Ahmed S, Naguib Ibrahim A, Draz Mohammed E, Zaazaa Hala E, Lashien Adel S
Cairo University, Faculty of Pharmacy, Analytical Chemistry Department, Kasr El-Aini St, 11562 Cairo, Egypt.
Beni-Suef University, Faculty of Pharmacy, Analytical Chemistry Department, 62111 Beni-Suef, Egypt.
J AOAC Int. 2018 Mar 1;101(2):427-436. doi: 10.5740/jaoacint.17-0069. Epub 2017 Aug 1.
Quantitative multicomponent analysis is considered an analytical goal to save time and cost in analysis. Hence, this work aimed to provide sensitive and selective UV-spectrophotometric, chemometric manipulation, and ultra-performance LC (UPLC) methods for the determination of well-known coformulated antiemetics used in pregnancy, namely pyridoxine HCl (PYR), meclozine HCl, and cyclizine. The developed UV-spectrophotometric methods are dual wavelength in ratio spectra and first derivative of the ratio spectra with which PYR was determined selectively at 290.8 nm, whereas the other drugs in a ternary mixture were determined from their ratio spectra using a spectrum of PYR as a divisor in 0.1 M HCl. An ecofriendly partial least-squares regression chemometric method was applied to raw UV absorbance data for the determination of the ternary mixture in a 218-355 nm range using a three-factor, three-level design with water as the green solvent. A gradient UPLC method was developed and successfully resolved the ternary mixture within 5 min. Different ratios of water (adjusted to pH 3 with phosphoric acid) and methanol were delivered at 0.5 mL/min as the mobile phase into a Hypersil Gold C18 column (50 × 2.1 mm, 1.9 µm). The developed methods were successfully applied to different pharmaceutical formulations containing the aforementioned drugs and validated according to the International Conference on Harmonization guidelines. The results obtained were reproducible and reliable and can be applied for routine analysis and QC in laboratories.
定量多组分分析被认为是一种可节省分析时间和成本的分析目标。因此，本研究旨在提供灵敏且具选择性的紫外分光光度法、化学计量学处理方法以及超高效液相色谱（UPLC）方法，用于测定孕期常用的复方止吐药，即盐酸吡哆醇（PYR）、盐酸美克洛嗪和赛克利嗪。所开发的紫外分光光度法包括比率光谱双波长法和比率光谱一阶导数法，利用该方法可在290.8 nm处选择性测定PYR，而三元混合物中的其他药物则以PYR的光谱为除数，在0.1 M盐酸中通过其比率光谱进行测定。将一种环保的偏最小二乘回归化学计量学方法应用于218 - 355 nm范围内的原始紫外吸光度数据，采用三因素、三水平设计，以水作为绿色溶剂来测定三元混合物。开发了一种梯度UPLC方法，并在5分钟内成功分离了三元混合物。以0.5 mL/min的流速将不同比例（用磷酸调节至pH 3）的水和甲醇作为流动相输送到Hypersil Gold C18柱（50×2.1 mm，1.9 µm）中。所开发的方法成功应用于含有上述药物的不同药物制剂，并根据国际协调会议指南进行了验证。所获得的结果具有可重复性和可靠性，可应用于实验室的常规分析和质量控制。
