Xun Xin-Jun
2010
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Journal
China Pharmacy
Abstract
OBJECTIVE:To develop GC method for the content determination of residual organic solvents in 4-(4-fluorophenyl)-6-isopropyl-2-[(N-methyl-N-methylsulfonyl)amido] pyriminl-5-yl-methanol,such as ethanol,acetone,dichloromethane,N-hexane,ethyl ether,methylbenzene and N,N-dimethylformamide.METHODS:Using dimethyl sulfoxide as the solvent and benzene as the internal standard,the determination was performed on a DB-624 capillary column with temperature program.FID was used as detector and nitrogen was used as carrier.The flow rate was set at 1.0 mL·min-1,and the inlet temperature was 220 ℃.The temperature of detector was set at 250 ℃ and the split ratio was 10:1.RESULTS:The linear ranges were 25.0~350.0 μg·mL-1 for ethanol,24.9~348.6 μg·mL-1 for acetone,3.2~44.8 μg·mL-1 for dichloromethane,1.6~22.4 μg·mL-1 for N-hexane,24.1~337.4 μg·mL-1 for ethyl ether,4.5~63.0 μg·mL-1 for methylbenzene and 5.4~75.6 μg·mL-1 for N,N-dimethylformamide (r0.995).The average recoveries ranged from 83.7% to 113.8%.Intra-day RSD was less than 4.2% and inter-day RSD was less than 4.6%.Ethanol,acetone,dichloromethane and DMF hadn't been detected in samples and the quantity of other solvents met the standard.CONCLUSION:The method is convenient,accurate and suitable for the determination of residual organic solvents in 4-(4-fluorophenyl)-6-isopropyl-2-[(N-methyl-N-methylsulfonyl)amido] pyriminl-5-yl-methanol.