摘要
Abstract
OBJECTIVE: To establish a method for the content determination of 5 kinds of residual organic solvents in thyroid tablets, I.e. Methanol, ethanol, acetone, ether and ethyl acetate. METHODS: Headspace capillary gas chromatography was adopted. The residual organic solvents were separated on DB-1 capillary column with FID detector. The carried gas was nitrogen. The injector temperature and detector temperature were controlled at 200℃ and 250℃, respectively. The column temperature was raised by program. The sample was dissolved in dimethyl sulfoxide. The containers of head-space injector were in equilibrium at 100℃ for 30 min, and the splitting-ratio was 10:1. RESULTS: The measured solvents were separated completely (r ranged 0.999 6~0.999 9). The detection limits were 0.6 μg·mL-1, 2.0 μg·mL-1, 1.0 μg·mL-1, 0.2 μg·mL-1, 0.1 μg·mL-1, respectively. The average recovery rates were 98.6%~100.3% (RSD=0.53%~1.32%). The residual organic solvents of 3 batches of samples were within standard range. CONCLUSION: The established method is simple, rapid, sensitive and accurate. It is suitable for the content determination of residual organic solvents in thyroid tablets.关键词
甲状腺片/顶空毛细管气相色谱法/有机溶剂/残留量Key words
Thyroid tablets/ Headspace capillary gas chromatography/ Organic solvents/ Residual分类
医药卫生
