Jilin Huakang Pharmaceutical Co. Ltd.

A method for the determination of residual solvents in agomelatine by GC was established.The detector was FID.The anal. column was an Agilent DB-WAX (30 m×0.32 mm, 0.25 μm) column.The injection temperature was 180°C and the detector temperature was 240°C.The column temperature was programmed raised.The initial temperature was 40°C, kept 10 min, then raised the temperature to 200°C with a rate of 20°C per min, and kept 5 min.The headspace vials equilibrium temperature was 80°C and the balance time was 30 min.Nitrogen was used as the carrier gas and N, N-dimethylformamide (DMF) was applied as the solvent media.The flow rate was 1.06 mL·min^-1.A good linear relationship was resp. obtained within the investigated concentration range of iso-Pr ether, THF, Et acetate, methanol, dichloromethane, ethanol and toluene.The average recovery was within the range of 97.7%-101.1% (n=9).The method is simple, sensitive and accurate, and can be used in the residual solvent detection for agomelatine.

The HPLC methods for determination of tanshinone II_A and salvianolic acid B in Xueshuan xinmaining tablets were established.C₁₈ column was used with methanol-water-glacial acetic acid (75:24:1) and methanol-acetonitrile 0.5% formic acid (30:9:61) as mobile phases at the detection wavelength of 270 nm and 286 nm, resp.The linear ranges of tanshinone II_A and salvianolic acid B were 3.44-34.40 μg (r = 0.9992) and 0.29-2.94 μg (r = 0.9999).The average recoveries of tanshinone II_A and salvianolic acid B were 98.80% (RSD = 0.72%) and 99.25% (RSD = 0.54%).

Bio-statistical methods for anti-factor Xa or anti-factor IIa of low-mol.-weight heparin (LMWH) evaluation were discussed.Chromogenic assay was used for bio-activity of LMWH by quantity response parallel line anal.Different bio-statistical methods and design were compared for exptl. reliability examination, potency and precision in anal. results.The differences of several bio-statistical methods and design by parallel line anal. were small and not statistically significant (P>0.05).Several bio-statistical methods and design could be used in validation of the anti-factor Xa or anti-factor IIa chromogenic assays for the potency assessment of LMWH by parallel line anal., when the results conforms to the standard