摘要
Abstract
Objective To establish a headspace gas chromatography ( HS-GC ) method for determination of 5 residual solvents in Estradiol Cypionate crude drug. Methods HS-GC method was performed by using Agilent DB-WAXetr column ( 30 m × 250 μm, 0. 5 μm ) , pro-grammed temperature, flow rate was 1. 5 mL/min, split ratio was 10:1, inlet temperature was 200 ℃, the detector was flame ionization detector, detecting temperature was 250 ℃. The bottles equilibrium temperature was 110 ℃, the equilibrium time was 30 min, and injec-tion volume was 1 mL. External standard method was used for quantitative analysis. Results The Linear range were 25~100 μg/mL ( r=0. 99949 ) for cyclopentyl propionyl chloride, 250~1000 μg/mL ( r=0. 99973 ) for acetic ether, 150~600 μg/mL ( r=0. 99968 ) for methanol, 250~1000 μg/mL ( r=0. 99973 ) for ethanol, 12. 5~50. 0 μg/mL ( r=0. 99958 ) for pyridine. The RSDs of precision were 1. 4%, 0. 7%, 1. 4%, 1. 4%, 2. 5% ( n=6 ) , respectively. The recoveries were 104. 55%( RSD=1. 19% ) , 93. 74% ( RSD=1. 40%) , 100. 94% ( RSD=1. 68% ) , 96. 42% ( RSD=1. 02% ) , 94. 52% ( RSD=3. 50% ) . The detection limit was 0. 04~0. 70 μg/mL and the quantitation limit was 0. 10 ~2. 5 μg/mL. Conclusion The method is simple, accurate and reproducible, which can be used for the determination of the 5 residual solvents in Estradiol Cypionate crude drug.关键词
环戊丙酸雌二醇/顶空气相色谱法/残留溶剂Key words
Estradiol Cypionate/headspace gas chromatography/residual solvent分类
化学化工
