Gallignani Máximo, Rondón Rebeca A, Ovalles José F, Brunetto María R
Laboratorio de Espectroscopia Molecular, Departamento de Química, Facultad de Ciencias, Universidad de Los Andes, Mérida 5101-A, Venezuela.
Departamento de Análisis y Control, Facultad de Farmacia y Bioanálisis, Universidad de Los Andes, Mérida 5101-A, Venezuela.
Acta Pharm Sin B. 2014 Oct;4(5):376-83. doi: 10.1016/j.apsb.2014.06.013. Epub 2014 Aug 8.
A Fourier transform infrared derivative spectroscopy (FTIR-DS) method has been developed for determining furosemide (FUR) in pharmaceutical solid dosage form. The method involves the extraction of FUR from tablets with N,N-dimethylformamide by sonication and direct measurement in liquid phase mode using a reduced path length cell. In general, the spectra were measured in transmission mode and the equipment was configured to collect a spectrum at 4 cm(-1) resolution and a 13 s collection time (10 scans co-added). The spectra were collected between 1400 cm(-1) and 450 cm(-1). Derivative spectroscopy was used for data processing and quantitative measurement using the peak area of the second order spectrum of the major spectral band found at 1165 cm(-1) (SO2 stretching of FUR) with baseline correction. The method fulfilled most validation requirements in the 2 mg/mL and 20 mg/mL range, with a 0.9998 coefficient of determination obtained by simple calibration model, and a general coefficient of variation <2%. The mean recovery for the proposed assay method resulted within the (100±3)% over the 80%-120% range of the target concentration. The results agree with a pharmacopoeial method and, therefore, could be considered interchangeable.
已开发出一种傅里叶变换红外导数光谱法(FTIR-DS)用于测定药物固体剂型中的呋塞米(FUR)。该方法包括通过超声处理用N,N-二甲基甲酰胺从片剂中提取FUR,并使用短程池在液相模式下直接测量。一般来说,光谱是在透射模式下测量的,设备配置为以4 cm⁻¹的分辨率和13 s的采集时间(共叠加10次扫描)采集光谱。光谱在1400 cm⁻¹至450 cm⁻¹之间采集。导数光谱用于数据处理和定量测量,使用在1165 cm⁻¹处发现的主要光谱带的二阶光谱的峰面积(FUR的SO2伸缩振动)并进行基线校正。该方法在2 mg/mL和20 mg/mL范围内满足了大多数验证要求,通过简单校准模型获得的测定系数为0.9998,总体变异系数<2%。所提出的测定方法的平均回收率在目标浓度的80%-120%范围内为(100±3)%。结果与药典方法一致,因此可以认为是可互换的。