Khan Muhammad N, Jan Muhammad N, Ullah Zafran
Department of Chemistry, Allama Iqbal Open University, Islamabad, Pakistan.
Department of Chemistry, Bacha Khan University, Charsadda, Pakistan.
Luminescence. 2023 Oct;38(10):1803-1813. doi: 10.1002/bio.4567. Epub 2023 Aug 21.
A responsive spectrofluorometric method was developed for the determination of sitagliptin phosphate using l-tyrosine as a fluorescence probe. The fluorescence intensity of l-tyrosine was quenched with sitagliptin phosphate. The fluorescence intensity was recorded at 307 nm using a 272 nm excitation wavelength. The calibration plot between fluorescence intensity and the concentration of drug was linear in the range of 0.1 to 2.0 mM with a good correlation value of 0.997. The limit of detection and quantification were established to be 3.7 × 10 and 1.23 × 10 mM, respectively. Commonly used excipients did not interfere with sitagliptin phosphate measurement. The proposed method was used to measure the sitagliptin phosphate in its standard type, dosage form, and biological samples. The percent recovery ranged from 97.41-103.36%. The static quenching was shown to be responsible for quenching as indicated by the Stern-Volmer plot. The method was validated using ICH guidelines and profitably applied for the content uniformity test, resulting in a high percent recovery and small relative standard deviation. The proposed approach is effortless, susceptible, selective, economic, and provides a high precision and accuracy, and can be used to determine sitagliptin phosphate in the pharmaceutical industry.
建立了一种以L-酪氨酸为荧光探针测定磷酸西格列汀的荧光分光光度法。L-酪氨酸的荧光强度被磷酸西格列汀猝灭。使用272nm激发波长在307nm处记录荧光强度。荧光强度与药物浓度之间的校准曲线在0.1至2.0mM范围内呈线性,相关系数为0.997。检测限和定量限分别为3.7×10和1.23×10mM。常用辅料不干扰磷酸西格列汀的测定。该方法用于测定磷酸西格列汀的标准品、剂型和生物样品。回收率在97.41-103.36%之间。如Stern-Volmer图所示,静态猝灭是导致猝灭的原因。该方法按照国际协调会议(ICH)指南进行了验证,并成功应用于含量均匀度测试,回收率高,相对标准偏差小。所提出的方法简便、灵敏、选择性好、经济,具有高精度和准确性,可用于制药行业中磷酸西格列汀的测定。