| A HPLC method for quantitative analysis of Levetiracetam was established. The experimental conditions for this method were the followings: cyano bonded silica column (250 mm×4.6 mm i.d. 5μm), methanol-50 mmol/L phosphate buffer fluid-Triethylamine (50:950:2) as mobile phase, UV detector fixed at 220 nm wavelength, the flow rate was 1.0 ml/min, the injection volume was 20μl, the column temperature was 25℃. Under the chromatographic conditions adopted, the appearance time of Levetiracetam was 7.568 min. The detection limit of Levetiracetam was 1.567×10-3 ng with the limit of quantitation of 5.224×10-3ng. The calibration curves was linear between 0.1621 g . L-1 and 0.2454 g . L-1 (r=0.9991). The method is suitable for the determination of levetiracetam.A practicable method for separation and quantitative analysis of dextro isomer in Levetiracetam was also established by HPLC. Methods: CHIRALPAK AD-H column (250 mm×4.6 mm i.d. 10μm) and the mobile phase of hexane-isopropyl alcohol (80:20) were used, wavelength of detection was 220 nm, injection volume was 20μL and the flow rate was 1.0 mL. min-1. By the chromatographic conditions, the separation of racemate could be finished within 10 mins, the resolution was 5.9, and the detection limit of dextro isomer was 4.112×10-6μg. L-1.A test method for the determination of three kind of residual organic solvents in levetiracetam by headspace gas chromatography was established. DB-WAX capillary column and FID-detector were adopted, external standard method was used for quantitative analysis. The proven results of optimized method were as follows: the average recoveries for acetone, ethyl acetate and dichloromethane were 97.45%, 97.17% and 94.47%, the standard curves for the three residual organic solvents were linear in the range of 0.05013 g .L-1-1.003 g.L-1(r=0.9997), 0.05011 g .L-1-1.002 g. L-1(r=0.9997) and 0.007000 g. L-10.1400 g. L-1(r=0.9888). The method is rapid, sensitive and simple.A practicable method for separation and determination of high molecular polymers in Cefonicid Sodium was found by HPLC with Sephadex G-10 column (10.0×300 mm). Mobile phase A was phosphate buffer fluid (0.025 mol . L-1, pH: 7.0), B was ultrapure water. The liquid chromatograph was equipped with a 254 nm detector. The flow rate was 0.7 mL . min-1 with injection volume being 20μl. The external standard method was used for quantitative analysis. The analysis method can improve the analysis efficiency significantly. |
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