ABSTRACT
OBJECTIVE:To establish a gas chromatography(GC)method for determination of seven residual solvents in clofarabine.METHODS:The capillary column was AT-1301;the carrier gas was nitrogen gas and the detector was FID.By temperature programming was applied for the column temperature with an initial temperature of 40 ℃,which rose to 80 ℃ with an increase rate of 7 ℃?min-1,then rose to 200 ℃(kept at this temperature for 2 min)with the increase rate of 20 ℃?min-1.The injector temperature was 250 ℃ and the detector temperature was 280 ℃.The sample was injected directly for determination of residual levels of methanol,acetonitrile,dichlormethane,t-butyl alcohol,ethyl acetate,n-heptane and acetic acid in 3 batches of clofarabine.RESULTS:All the organic solvents were effectively separated and they showed good linearity within a concentration range(r=0.999 41～0.999 93)with average recovery rate ranged from 96.5% to 102.4%(RSDs of all were less than 4.0%).7 kinds of organic solvents in 3 batches of samples were all up to the standard specified in Chinese Pharmacopeia.CONCLUSION:The method is sensitive,accurate and reliable,and it is applicable for the determination of the residual solvents in clofarabine.
ABSTRACT
OBJECTIVE: To determine the residual levels of 4 organic solvents(methanol,alcohol,ether and acetone) in the raw material of medicinal sodium ozagrel by capillary gas(GC) chromatography.METHODS: The determination was performed using hydrogen flame ionization detector,AB-CarboWax with nitrogen gas as carrier gas using temperature programming for the column temperature.The sample size was 1 ?L,the temperature of the detector was 280 ℃,the temperature for sample injection was 250 ℃,the flow rate of carrier gas was 1 mL?min-1,and the flow rate of the hydrogen gas was 40 mL?min-1.RESULTS: The linear ranges of methanol was 0.037 5～3 mg?mL-1,alcohol,ether and acetone were 0.062 5～5 mg?mL-1,respectively,their average recoveries ranged from 98.07% to 99.12% with RSD being 0.34%～0.65%.Their lowest detection limits were all less than 3.125 ?g?mL-1,which were undetected for all the samples.CONCLUSIONS: The method is simple,sensitive and accurate,and it can be used for the determination of the residual levels of organic solvents in the raw medicinal of sodium ozagrel.
ABSTRACT
OBJECTIVE: To establish a CGC method for the determination of pyridine in Potassium Dehydroandrograpol-ide Succinate. METHODS: The determination was performed on HP-INNOWAX capillary with column temperature at 100℃. The FID detector was used and the carrier gas was nitrogen. RESULTS:The linear range of Pyridine was 2.46～39.3?g?mL-1 and the average recovery was 98.07%,RSD=4.00(n=9).Its detection limit was 0.2?g?mL-1.CONCLUSION: The method is accurate and rapid, and applicable for the determination of the residual level of Pyridine in Potassium dehydroandrograpolide succinate.