title: Development and Validation of Miglitol and Its Impurities by RP-HPLC and Characterization Using Mass Spectrometry Techniques.
abstract: Alpha glucoside inhibitors used to treat type-2 diabetes mellitus (DM) are likely to be safe and effective. These agents are most effective for postprandial hyperglycemia. Miglitol is a type of drug used to treat type-2 DM. A simple, selective, linear, precise and accurate reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for a related substance of miglitol and its identification, and characterization was done by different mass spectrometry techniques. The gradient method at a flow rate of 1.0 mL/min was employed on a prevail carbohydrate ES column (250 × 4.6 mm, 5 μm particle size) at a temperature of 35 °C. Mobile phase A consisted of 10 mM dipotassium hydrogen orthophosphate adjusted to pH 8.0 using concentrated phosphoric acid and mobile phase B consisted of acetonitrile. The ultraviolet detection wavelength was 210 nm and 20 μL of the sample were injected. The retention time for miglitol was about 24.0 min. Forced degradation of the miglitol sample was conducted in accordance with the International Conference on Harmonisation (ICH) guidelines. Acidic, basic, neutral, and oxidative hydrolysis, thermal stress, and photolytic degradation were used to assess the stability-indicating the power of the method. Substantial degradation was observed during oxidative hydrolysis. No degradation was observed under the other stress conditions. The method was optimized using samples generated by forced degradation and sample solutions spiked with impurities and epimers. Good resolution of the analyte peak from peaks, corresponding to process-related impurities, epimers and degradation products, was achieved and the method was validated as per the ICH guidelines. The method can successfully be applied for routine analysis of miglitol.
authors.affiliation: Analytical Research, Custom Pharmaceutical Services, Dr. Reddy's Laboratories Ltd., Bollaram Road, Miyapur, Hyderabad 500049, India. balakumarank@drreddys.com.|Centre for Chemical Sciences & Technology, Institute of Science and Technology, Jawaharlal Nehru Technological University, Kukatpally, Hyderabad 500085, India. balakumarank@drreddys.com.
authors.forename: Kesavan
authors.initials: K
authors.lastname: Balakumaran
authors.affiliation: Analytical Research, Custom Pharmaceutical Services, Dr. Reddy's Laboratories Ltd., Bollaram Road, Miyapur, Hyderabad 500049, India. mosesbabuj@drreddys.com.
authors.forename: Mosesbabu
authors.initials: M
authors.lastname: Janagili
authors.affiliation: Analytical Research, Custom Pharmaceutical Services, Dr. Reddy's Laboratories Ltd., Bollaram Road, Miyapur, Hyderabad 500049, India. nagarajurajana@drreddys.com.
authors.forename: Nagaraju
authors.initials: N
authors.lastname: Rajana
authors.affiliation: Analytical Research, Custom Pharmaceutical Services, Dr. Reddy's Laboratories Ltd., Bollaram Road, Miyapur, Hyderabad 500049, India. psbabu8277@gmail.com.
authors.forename: Sureshbabu
authors.initials: S
authors.lastname: Papureddy
authors.affiliation: Centre for Chemical Sciences & Technology, Institute of Science and Technology, Jawaharlal Nehru Technological University, Kukatpally, Hyderabad 500085, India. jayashreeanireddy@gmail.com.
authors.forename: Jayashree
authors.initials: J
authors.lastname: Anireddy
keywords: DNJ (1-deoxynojirimycin); forced degradation; high performance liquid chromatography; mass spectrometry; miglitol; reverse phase liquid chromatography; stability-indicating methods