Development And Verification Of Egliaegin Analysis Method

Eggliflozin pyroglutamate is a sodium-glucose cotransporter(SGLT-2)inhibitor approved by the FDA for the treatment of type Ⅱ diabetes.It is safe to take,well tolerated,and has few adverse reactions.At present,although there are a small number of reports on the analysis and detection methods of Egliflozin,these methods do not have specific analysis methods for related substances and content.At the same time,there is no relevant report concerning the analysis and detection method of Eggliflozin residual solvent.This thesis first introduces the background of the subject of this thesis,including a summary of the onset of diabetes and the treatment plan,puts forward the advantages of Egligliflozin pyroglutamate in the treatment of diabetes,and focuses on SGLT-2 The role of inhibitors;secondly,it summarizes the general rules and requirements for drug quality research,and provides references for new drug research;then studies the physical and chemical properties of eggliflozin,and develops methods for the analysis and detection of eggliflozin related substances.It has been verified to provide a reference for the further production,testing and use of the drug.It is divided into the following four parts:The first part introduces the overview of SGLT-2 inhibitors of diabetes,outlines the general rules and requirements of drug quality research,and summarizes the current research status of Egligliflozin analysis methods.e second part first studies the physicochemical properties of eggliflozin,including appearance,melting point,solubility and so on.Next,the analytical method for Eggliflozin was developed and verified,and the chromatographic conditions suitable for the actual detection process of Eggliflozin were determined:Agilent Proshell 120 EC C18(5×150mm,4.6μm)chromatographic column was adopted,Column temperature 35℃,flow rate 1 mL·min-1,detection wavelength 210 nm,gradient elution method:buffer-acetonitrile(65%-3 5%)(v/v)isocratic elution for 12 min,organic phase Acetonitrile was increased to 80%in 12 to 18 minutes,and then isocratic for 12 minutes.Through method verification,the results show that the method is stable,accurate and highly reproducible.Among them,the linear regression equation of Egliflozin related substances in the concentration range of 0.0506 μg·mL-1～1.012μg·mL-1 is:y=24.780x-0.0692(R2=0.9987),which has a good linear relationship,and the content is 0.1625 The linear regression equation within the concentration range of-0.2413 mg·mL-1 is y=24281x+79.963(R2=0.9991),which has a good linear relationship.Chromatographic conditions for the detection of residual solvents of Eggliflozin:use Agilent DB-624 30mm 0.53mm 3.0μm chromatographic column,start temperature 40℃,keep for 15min,then increase to 210℃ at a rate of 30℃/min,keep for 5min.The inlet temperature is 240℃,the detector temperature:250℃,carrier gas:N2,flow rate:1.0 mL/min,split ratio:100:1.Similarly,by verifying the method,the results show that the method is stable,accurate and highly reproducible.The third part is to study the stability of eggliflozin.Firstly,the influencing factors in 5 days and 10 days are investigated,and then the stability changes of eggliflozin in the early 0-6 months are investigated.It is found that the drug has some problems in some aspects.Stable performance.The fourth part summarizes the full text.