Dongala Thirupathi, Katari Naresh Kumar, Palakurthi Ashok Kumar, Jonnalagadda Sreekantha B
Aurex Laboratories LLC, NJ, USA.
Department of Chemistry, GITAM deemed to be University, Hyderabad, Telangana, India.
Biomed Chromatogr. 2019 Nov;33(11):e4641. doi: 10.1002/bmc.4641. Epub 2019 Aug 8.
A novel generic reverse phase high performance liquid chromatography (RP-HPLC) method is developed and validated for simultaneous determination of seven pharmaceutically active ingredients, namely, acetaminophen, dextromethorphan, doxylamine, phenylephrine, guaifenesin, caffeine and aspirin. All seven ingredients were quantified in soft gel, syrup and tablet formulations of the over-the-counter US-marketed products, as per the guidelines of the International Conference on Harmonization. The separation was achieved in a 16 min run time on an Agilent Zorbax Phenyl column using a gradient method with two mobile phases. Mobile phase A was 0.15% trifluoro acetic acid in purified water and while mobile phase B was a mixture of acetonitrile and methanol (750:250 v/v) with 0.02% trifluoro acetic acid. The flow rate was 1.0 mL min and injection volume was 10 μL. Detection was performed at 280 nm using a photodiode array detector. As part of the method validation, specificity, linearity, precision and recovery parameters were verified. The concentration and area relationships were linear (R > 0.999), over the concentration ranges 20-120 μg mL for acetaminophen, 75-450 μg mL for dextromethorphan, 31.25-187.5 μg mL for doxylamine, 25-150 μg mL for phenylephrine, 25-150 μg mL for aspirin, 6.5-39 μg mL for caffeine and 12-72 μg mL for guaifenesin. The relative standard deviations for precision and intermediate precision were <1.5%. The proposed RP-HPLC generic method is applicable for routine analysis of cold and cough over-the-counter products.
开发并验证了一种新型通用反相高效液相色谱（RP-HPLC）方法，用于同时测定七种药物活性成分，即对乙酰氨基酚、右美沙芬、多西拉敏、去氧肾上腺素、愈创甘油醚、咖啡因和阿司匹林。按照国际协调会议的指导方针，对美国市场上非处方产品的软胶囊、糖浆和片剂剂型中的所有七种成分进行了定量分析。使用含有两种流动相的梯度方法，在Agilent Zorbax苯基柱上于16分钟的运行时间内实现了分离。流动相A为纯化水中含0.15%的三氟乙酸，而流动相B是乙腈和甲醇（750:250 v/v）的混合物并含有0.02%的三氟乙酸。流速为1.0 mL/min，进样体积为10 μL。使用光电二极管阵列检测器在280 nm处进行检测。作为方法验证的一部分，对特异性、线性、精密度和回收率参数进行了验证。在对乙酰氨基酚浓度范围为20 - 120 μg/mL、右美沙芬为75 - 450 μg/mL、多西拉敏为31.25 - 187.5 μg/mL、去氧肾上腺素为25 - 150 μg/mL、阿司匹林为25 - 150 μg/mL、咖啡因6.5 - 39 μg/mL以及愈创甘油醚为12 - 72 μg/mL时，浓度与面积关系呈线性（R＞0.999）。精密度和中间精密度的相对标准偏差＜1.5%。所提出的RP-HPLC通用方法适用于感冒和咳嗽非处方产品的常规分析。
