Determination of Residual Solvents in Raw Material Drug of Cefotiam Hexetil Hydrochloride by Gas Chromatography with Head-space Sampling / 医药导报

ABSTRACT

Objective To establish a method of gas chromatography with head-space sampling for determination of five residual solvents ( acetone, ethyl acetate, isopropanol, dichloromethane, acetonitrile ) in raw material drug of cefotiam hexetil hydrochloride. Methods Agilent DB-624 capillary column(30 m×0.53 mm,3.0 μm)was used,with FID served as detector and DMF as the solvent. Results Linear relationships were obtained for the 5 residual solvents in their respective concentration ranges ( r=0.999 6-0.999 9,n=5) ,and the detection range was from 0.071 to 0.847μg. The stabilities measured as relative standard deviations ( RSD) for the 5 residual solvents were from 0.40% to 2.12% ( n=3) . The average recovery rates were 99.03% to 103.33%,and RSD were 0.54% to 3.41% ( n=3) . Conclusion The method is simple,sensitive and accurate for the residual solvent analysis in raw material drug of cefotiam hexetil hydrochloride.