Determination of Residue Levels of Organic Solvents in Docetaxel by Head Space GC

OBJECTIVE:To established a method for determination of residue levels of 8 organic solvents including methanol and dichlormethane in docetaxel crude drug. METHODS: GC-MS was employed to identify the peaks of two unknown residual solvents in docetaxel,and head space GC was employed to determined 8 organic solvents. The chromatographic condition was as follows: the chromatographic column was HP-5;the carrier gas was nitrogen gas;the detector was flame ionization detector which was kept at 250 ℃;the injector temperature was 180 ℃. The column temperature was programmed raised;the flow rate was 1.7 mL·min-1;the split ratio was 1∶10;the sample was injected by head space injection with an injection volume of 1.0 mL. RESULTS: The unknown residual solvents in docetaxel were determined as 3-methylpentane and methylcyclopentane. The 8 solvents showed good linear relationship within a certain concentration range (r0.997 3) and their average recovery rates were all above 91.3% (RSD3.8%,n=5). CONCLUSION: This method is sensitive,accurate and reliable and it can be applied for the determination of residue level of organic solvents in docetaxel.