Determination of Organic Solvent Residues in Testosterone Cypionate / 医药导报

ABSTRACT

Objective To establish a headspace GC method for the determination of residual organic solvents in testosterone cypionate. Methods The residual organic solvents were determined by GC with DB-WAX capillary colum(30 m× 0. 32 mm,0. 25 μm)and FID detector at 230℃,using high purity nitrogen as the carrier gas by headspace sampling. The flow rate was 1. 5 mL·min-1 ,the split ratio was 201,the temperature of injection port was 220℃,the headspace heating temperature was 70 ℃,and the headspace balance time was 40 mins. The content of residues was calculated by using n-propanol as the internal standard. Results Four residual solvents were completely separated. There were good linearity for m-ethanol,ethanol,benzene and pyridinein in the ranges of 4. 17-2. 50×103 μg·g-1(R=0. 999 9),4. 18-2. 51×103 μg·g-1(r=0. 999 6),0. 84-172 μg·g-1 (r=0. 998 1),and 2. 95-1. 77×103μg·g-1(r=0. 999 9),respectively. The detection limit was 2.08,1. 23,0.28,and 0. 87 μg·g-1,respectively. The average recovery of methanol,ethanol,benzene and pyridinein was 102. 2%(RSD=4. 0%),99. 6%(RSD=1. 9%),112. 6(RSD=5. 6%),and 98. 9%(RSD=1. 6%),respectively. Conclusion This method is reliable,sensitive, accurate and can be used for the determination of residual organic solvents in testosterone cypionate.