Itigimatha Nandeesha, Chadchan Kailash S, Yallur Basappa C, Hadagali Manjunatha D
Visvesvaraya Technological University, Ramaiah Institute of Technology, Department of Chemistry, Bangalore, India
BLDEA's V.P. Dr. P.G. Halakatti College of Engineering and Technology, Department of Chemistry, Karnataka, India
Turk J Pharm Sci. 2022 Apr 29;19(2):213-219. doi: 10.4274/tjps.galenos.2021.55381.
Simple, novel and selective reverse phase-high performance liquid chromatography (RP-HPLC) and ultraviolet (UV) spectroscopic methods have been developed and optimized for the determination of remogliflozin etabonate (RMZ) in bulk and dosage forms. In the HPLC method, the principal peak and internal standard peak were eluted separately at different retention times (RT) with the chromatographic conditions such as, mobile phase consisting of 0.02 M ammonium acetate buffer (pH was adjusted to 4.0 by 1.0 M ortho phosphoric acid), acetonitrile and tetrahydrofuran in the ratio 50:45:05, respectively (v/v) and the stationary phase used was C18, 5 μm, 4.6 mm x 250 mm kromasil column. The flow rate was 2.0 mL min, sample injection volume was 10 μL, and the wavelength of detection was fixed at 228 nm. In case UV spectroscopic method, the RMZ was diluted with pure ethanol. The RMZ showed a maximum absorbance at 228 nm. Hence throughout analysis 228 nm was used for the determination of RMZ. The RT of RMZ and internal standard, atorvastatin (ATST) were 6.2 min and 7.0 min, respectively. The resolution between the peaks was found to be more than 2.0. The total run time was fixed at 10 min. The linearity range for RP-HPLC method was found to be 10 μg mL to 50 μg mL, at a fixed concentration of ATST. The linearity range for the UV spectroscopic method was found to be in the range of 100 to 250 μg mL. Regression coefficients (R2) were found above 0.999 for both of the techniques. The limit of detection and quantification for RMZ were found to be 1.0 μg mL-1 and 3.5 μg mL respectively, in RP-HPLC method and 10.0 μg mL and 40 μg mL, respectively, in UV spectroscopic method. The developed methods were found to be simple, accurate, reproducible, and precise. The RMZ can be analyzed in dual techniques, ., chromatographic and UV spectroscopic methods for its routine analysis.
已开发并优化了简单、新颖且具选择性的反相高效液相色谱法（RP-HPLC）和紫外（UV）光谱法，用于测定原料药及制剂中的瑞格列净乙酯（RMZ）。在HPLC法中，主峰和内标峰在不同保留时间（RT）分别洗脱，色谱条件如下：流动相由0.02 M醋酸铵缓冲液（用1.0 M正磷酸将pH调至4.0）、乙腈和四氢呋喃按50:45:05的比例（v/v）组成，所用固定相为C18、5μm、4.6 mm×250 mm的科马西色谱柱。流速为2.0 mL/min，进样体积为10μL，检测波长固定在228 nm。在UV光谱法中，RMZ用无水乙醇稀释。RMZ在228 nm处有最大吸收。因此，在整个分析过程中，228 nm用于RMZ的测定。RMZ和内标阿托伐他汀（ATST）的保留时间分别为6.2 min和7.0 min。发现峰之间的分离度大于2.0。总运行时间固定为10 min。在ATST固定浓度下，RP-HPLC法的线性范围为10μg/mL至50μg/mL。UV光谱法的线性范围为100至250μg/mL。两种技术的回归系数（R2）均高于0.999。在RP-HPLC法中，RMZ的检测限和定量限分别为1.0μg/mL-1和3.5μg/mL，在UV光谱法中分别为10.0μg/mL和40μg/mL。所开发的方法简单、准确、可重现且精密。RMZ可通过两种技术进行分析，即色谱法和UV光谱法，用于其常规分析。
