Bui Van Trung, Doan Cao Son, Tong Thi Thanh Vuong, Le Dinh Chi
National Institute of Drug Quality Control, Ministry of Health, Hanoi, Vietnam.
Department of Analytical Chemistry and Toxicology, Hanoi University of Pharmacy, Hanoi, Vietnam.
J Anal Methods Chem. 2021 Feb 13;2021:6616728. doi: 10.1155/2021/6616728. eCollection 2021.
A simple, easy-to-implement, and green infrared spectroscopic method was developed and validated for the quantitative determination of sildenafil citrate in tablets of unknown manufacturing formula. Homogenized tablet powder with known mass content (%, m/m) of sildenafil citrate was mixed with paracetamol to form standard mixtures with different percentages of sildenafil citrate on the total quantity of sildenafil citrate and paracetamol (designated as R). Unknown tablet samples were finely ground and mixed with paracetamol to form test mixtures having values about 50%. Infrared spectra of standard mixtures, measured in attenuated total reflectance mode, in the wavenumber zone from 1800 cm to 1300 cm were selected and processed by partial least square regression to form the calibration model for quantitation of sildenafil citrate in unknown samples. Spectral responses of test mixtures and the calibration model were used to determine the exact mass content (%, m/m) of sildenafil citrate in the powder of unknown tablet samples. The method was fully validated in terms of linearity, precision, and accuracy according to the requirements of current guidelines and was proved as reliable and suitable for the intended application.
开发并验证了一种简单、易于实施且绿色的红外光谱法，用于定量测定未知生产配方片剂中的枸橼酸西地那非。将具有已知质量含量（%，m/m）的枸橼酸西地那非的均质片剂粉末与对乙酰氨基酚混合，以形成枸橼酸西地那非在枸橼酸西地那非和对乙酰氨基酚总量中具有不同百分比的标准混合物（记为R）。将未知片剂样品精细研磨并与对乙酰氨基酚混合，以形成 值约为50%的测试混合物。选择在衰减全反射模式下在1800 cm至1300 cm波数范围内测量的标准混合物的红外光谱，并通过偏最小二乘回归进行处理，以形成用于定量未知样品中枸橼酸西地那非的校准模型。测试混合物的光谱响应和校准模型用于确定未知片剂样品粉末中枸橼酸西地那非的确切质量含量（%，m/m）。根据现行指南的要求，该方法在线性、精密度和准确度方面得到了充分验证，并被证明可靠且适用于预期应用。
