Fernandes Tânia A P, Aguiar João P, Fernandes Ana I, Pinto João F
CiiEM - Centro de Investigação Interdisciplinar Egas Moniz, Instituto Superior de Ciências da Saúde Egas Moniz, Campus Universitário-Quinta da Granja, Monte de Caparica, 2829-511 Caparica, Portugal.
iMed.UL - Dep. Tecnologia Farmacêutica, Faculdade de Farmácia, Universidade de Lisboa, Av. Prof. Gama Pinto, 1649-003 Lisboa, Portugal.
J Pharm Anal. 2017 Dec;7(6):401-405. doi: 10.1016/j.jpha.2017.07.005. Epub 2017 Jul 13.
A simple, accurate and sensitive high-performance liquid chromatography (HPLC) method was developed, validated and applied to the determination of either theophylline or paracetamol in milk-based samples. The method allowed drug quantification in fresh and powdered milk with a relatively short run time of analysis and it was also successfully applied to the quantification of the drugs in solid dosage forms intended for pediatric use. Moreover, the main significant advantages over other published works are the simplicity of the sample preparation, reduced assay time and sample loss. The method meets the International Conference on Harmonization guideline for analytical methods validation regarding specificity, linearity, accuracy, precision, specificity and robustness as required by health authorities and applied by industry while designing and marketing new drug products. The technique encompasses the separation of the analytes with a reverse phase C column under isocratic conditions and UV detection at 272 nm and 243 nm, respectively, for theophylline and paracetamol. The lower limit of quantification for both drugs was determined as 0.2 µg/mL and the between-batch accuracy was approximately 99.7%. This HPLC method allows quantification of theophylline and paracetamol in milk matrices and it can be applied in the design, development and production of milk-based pediatric dosage forms.
开发并验证了一种简单、准确且灵敏的高效液相色谱（HPLC）方法，并将其应用于测定乳基样品中的茶碱或对乙酰氨基酚。该方法能够在相对较短的分析运行时间内对新鲜牛奶和奶粉中的药物进行定量，并且还成功应用于儿科用固体剂型中药物的定量。此外，与其他已发表的研究相比，该方法的主要显著优势在于样品制备简单、分析时间缩短以及样品损失减少。该方法符合国际协调会议（ICH）关于分析方法验证的指导原则，满足卫生当局和制药行业在设计和销售新药产品时对特异性、线性、准确性、精密度、专属性和稳健性的要求。该技术包括在等度条件下用反相C柱分离分析物，并分别在272 nm和243 nm处对茶碱和对乙酰氨基酚进行紫外检测。两种药物的定量下限均确定为0.2 μg/mL，批次间的准确度约为99.7%。这种HPLC方法能够对乳基质中的茶碱和对乙酰氨基酚进行定量，可应用于基于牛奶的儿科剂型的设计、开发和生产。
