Determination of Residual Organic Solvents in Antitumor di-phenyl-di-(2,4-dichlorobenzohydroxamato)tin by Capillary Gas Chromatography

摘要

To determine the residual organic solvents (methanol, dichloromethane, normal hexane) in antitumor crude drug di-phenyl-di-(2,4-dichlorobenzohydroxamato)tin(DPDCT), capillary gas chromatography (GC) method was established. The HP-5 (30 m×320μm×0.25μm) capillary column and flame ionization detector (FID) detector were adopted. The carrier gas was nitrogen with flow rate 5.08 ml·min~(-1). The column temperature was 50.0°C and column pressure was 20.00 psi. The distributary ratio was 20:1. 1, 2-dichloroethane was used as the internal standard substance while toluene as the solvent to determine the residual organic solvents. The calibration curves for methanol, dichloromethane and normal hexane are linear in the rang of 180.6～481.5μg·ml~(-1)(r~2 = 0.9974), 35.78～95.40μg·ml~(-1)(r~2 = 0.9950), 17.82～47.52μg·ml~(-1)(r~2 = 0.9995), respectively. The average recoveries of methanol, dichloromethane and normal hexane are 100.4% (RSD=1.8%), 100.3% (RSD=1.7%), 99.6% (RSD=1.5%), respectively. The method is a simple and accurate method with high sensitivity and repeatability. It is suitable for the residual solvent determination of antitumor DPDCT.