Gurrala Sunitha, Raj Shiva, Cvs Subrahmanyam, Anumolu Durga Panikumar, Naraparaju Swathi, Nizampet Harika
Osmania University, University College of Technology, Department of Pharmacy, Hyderabad, India
Osmania University, University College of Science, Department of Chemistry, Hyderabad, India
Turk J Pharm Sci. 2022 Feb 28;19(1):9-18. doi: 10.4274/tjps.galenos.2021.93195.
Design of experiments assisted spectrophotometric methods have been established for the quantification of saxagliptin in pharmaceutical formulation charge transfer complexation and Schiff's base formation.
Box-Behnken design was exploited in method-1, involved the measurement of absorbance of green/blue-colored complex (at 600 nm), formed by the reaction of saxagliptin with 3-methyl-2-benzothiazolinone hydrazone in the presence of ferric chloride. The central composite design was employed in method-2, involved the determination of absorbance of Ruhemann's purple (at 585 nm), formed by the reaction of the primary amine group of saxagliptin with ninhydrin reagent in presence of sodium hydroxide. Optimization of reaction variables namely, reagent concentration (A), oxidizing agent/alkalinity (B) and reaction/heat time (C) was performed through response surface methodology for the response (Y) absorbance of colored compound. The reliability of both methods was investigated through validation as International Council for Harmonisation guidelines.
Saxagliptin executed linearity in the concentration range of 0.01-0.25 μg/mL and 1-10 μg/mL by method-1 and 2. A high value of molar absorptivity, low values of Sandell's sensitivity and limit of detection/limit of quantification divulges the good sensitivity methods. The % assay of saxagliptin in the marketed formulation was found to be 100.27 and 99.86 by method-1 and method-2, respectively.
The proposed eco-friendly and economical methods can be routinely employed in quality control for the analysis of saxagliptin in the pharmaceutical dosage forms.
建立了实验辅助分光光度法，用于药物制剂中沙格列汀的定量分析，包括电荷转移络合和席夫碱形成。
方法1采用Box-Behnken设计，涉及测量沙格列汀与3-甲基-2-苯并噻唑啉酮腙在氯化铁存在下反应形成的绿色/蓝色络合物（在600nm处）的吸光度。方法2采用中心复合设计，涉及测定沙格列汀的伯胺基团与茚三酮试剂在氢氧化钠存在下反应形成的鲁赫曼紫（在585nm处）的吸光度。通过响应面法对反应变量即试剂浓度（A）、氧化剂/碱度（B）和反应/加热时间（C）进行优化，以获得有色化合物的响应（Y）吸光度。按照国际协调理事会指南通过验证研究了两种方法的可靠性。
方法1和方法2中，沙格列汀在0.01-0.25μg/mL和1-10μg/mL的浓度范围内呈线性。高摩尔吸光率值、低桑德尔灵敏度值以及低检测限/定量限表明这些方法具有良好的灵敏度。通过方法1和方法2测定市售制剂中沙格列汀的含量分别为100.27%和99.86%。
所提出的环保且经济的方法可常规用于药物剂型中沙格列汀分析的质量控制。
