Abstract
Objective To develop a headspace gas chromatography for the determination of 8 residual solvents in alpha lipoic acid and to ensure the quality accordance with the requirements of the medical. Methods After being dissolved with DMSO, the eight residual solvents including alcohol, acetone, n-hexane, ethyl acetate, cyclohexane, methylbenzene, chloroform, 1, 2- dichloroethane in alpha lipoic acid were separated by GC on a capillary column ( SPB-5, 60 m × 0. 53 mm, 3. 0 μm ) with a mobile phase of nitrogen. And the quan-tities of the 8 residual solvents in alpha lipoic acid were calculated respectively. Results The calibration curves for alcohol, acetone, n-hexane, ethyl acetate, cyclohexane, methylbenzene, chloroform, 1, 2-dichloroethane were linear over the range of 123. 9-1 983 g/mL, 126. 8-2 029 g/mL, 7. 284-116. 5 g/mL, 12. 89-1 031 g/mL, 95. 32-1 525 g/mL, 27. 05-432. 8 g/mL, 1. 268-20. 29 g/mL, 0. 139 9-1. 399 g/mL( r=0. 999 0-1. 000 0), respectively. The average recovery rates were 103. 3% , 95. 9% , 93. 1% , 95. 3% , 97. 5%, 95. 2%, 93. 3%, 91. 1%, RSD were 0. 8%, 0. 7%, 1. 1%, 0. 9%, 1. 1%, 1. 0%, 1. 4%, 1. 0%( n=9 ) , respectively. And the LOD were 15. 37 μg/g, 0. 86 μg/g, 0. 38 μg/g, 8. 30 μg/g, 0. 090 μg/g, 1. 59 μg/g, 1. 27 μg/g, 0. 12 μg/g, respactively. Conclusion The method is sensitive, accurate and convenient with good resolution, which can be applied to control the quality of alpha lipoic acid.关键词
硫辛酸/残留溶剂/顶空毛细管气相色谱法Key words
alpha lipoic acid/residual solvent/HS-GC分类
医药卫生
