Résumé
Objective To establish a HPLC method for determination of 18β-isomer in magnesium isoglycyrrhizinate. Methods The determination was performed by Agilent Extend-C18 column ( 4. 6 mm × 250 mm, 5 μm ) . Mobile phase consisted of 0. 1 mol·L-1 potassium dihydrogen phosphate buffer solution ( adjusted to pH 7. 0 with potassium hydroxide )-acetonitrile (80︰20) at the flow rate of 1.0 mL·min-1. The column temperature was 30 ℃, and the detection wavelength was set at 250 nm. Results The resolution of magnesium isoglycyrrhizinate and 18β-isomer was greater than 2.0. The linear range of them was 0.41-2.46μg·mL-1( r=0.9998) , the detection limit was 0.21 ng, and the average recovery were 100.2%,99.1%, 110.2%,RSD were 0.9%,0.1%,0.2%(n=3). Conclusion The method is simple and accurate, and can be used for determination of 18β-isomer in magnesium isoglycyrrhizinate.
Résumé
Objective To establish a HPLC method for determination of 18β-isomer in magnesium isoglycyrrhizinate. Methods The determination was performed by Agilent Extend-C18 column ( 4. 6 mm × 250 mm, 5 μm ) . Mobile phase consisted of 0. 1 mol·L-1 potassium dihydrogen phosphate buffer solution ( adjusted to pH 7. 0 with potassium hydroxide )-acetonitrile (80︰20) at the flow rate of 1.0 mL·min-1. The column temperature was 30 ℃, and the detection wavelength was set at 250 nm. Results The resolution of magnesium isoglycyrrhizinate and 18β-isomer was greater than 2.0. The linear range of them was 0.41-2.46μg·mL-1( r=0.9998) , the detection limit was 0.21 ng, and the average recovery were 100.2%,99.1%, 110.2%,RSD were 0.9%,0.1%,0.2%(n=3). Conclusion The method is simple and accurate, and can be used for determination of 18β-isomer in magnesium isoglycyrrhizinate.
Résumé
Objective To establish a method for simultaneous determination of petroleum ether (60-90 ℃),ethyl acetate,ethanol and pyridineas residual organic solvents in imatinib mesylate API. Methods Capillary gas chromatography was adopted.The determination was performed on DB-WAX capillary column with FID detector.The injector temperature was 180 ℃and the temperature of FID was 200 ℃ by temperature programming with nitrogen serving as carrier gas at a flow rate of 5 mL·min-1.The injection volume was 1 μL.With N,N-dimethylformamide(DMF) serving as solvent,four kinds of organic solvent residues in the samples were calculated by external standard method. Results The four kinds of organic solvent were completely separated under the established chromatographic condition.A good linearity was obtained in the concentration ranges of them (r=0.999 8-0.999 9).The sampling precisions (RSDs) were less than 2.0%(n=5).The average recovery rates of ethyl acetate,ethanol and pyridine were 97%-101%and that of petroleum ether was 88.7%(RSD<2.0%,n=5).The limits of detection for them were 0.58,0.42,0.18 and 0.61 ng respectively(S/N=3:1).The limits of quantification for them were 1.8,2.1,0.5 and 2.5 ng,respectively (S/N=10:1). Conclusion The method is simple,sensitive,accurate and reliable.
Résumé
Though all the marketed drugs of dipeptidyl peptidase IV inhibitors are structurally different, their inherent correlation is worthy of further investigation. Herein we rapidly discovered a novel DPP-IV inhibitor 8g (IC50 = 4.9 nmol.L-1) which exhibits as good activity and selectivity as the market drugs through scaffold hopping and drug splicing strategies based on alogliptin and linagliptin. This study demonstrated that the employment of classic medicinal chemistry strategy to the marketed drugs with specific target is an efficient approach to discover novel bioactive molecules.