摘要
目的建立同时测定硫辛酸原料药中乙醇、丙酮、正己烷、乙酸乙酯、环己烷、甲苯、三氯甲烷和1,2-二氯乙烷8种残留溶剂含量的顶空毛细管气相色谱法,以保证硫辛酸的质量满足药用要求。方法采用顶空进样系统程序升温法,以FID为检测器,以5%二苯基-95%二甲基聚硅氧烷为固定液的毛细管柱为色谱柱（SPB-5,60 m×0.53 mm,3.0μm）。结果乙醇、丙酮、正己烷、乙酸乙酯、环己烷、甲苯、三氯甲烷和1,2-二氯乙烷质量浓度分别在123.9～1 983μg/m L,126.8～2 029μg/m L,7.284～116.5μg/m L,12.89～1 031μg/m L,95.32～1 525μg/m L,27.05～432.8μg/m L,1.268～20.29μg/m L,0.139 9～1.399μg/m L范围内与峰面积线性关系良好（r在0.999 0～1.000 0）;平均回收率分别为103.3%,95.9%,93.1%,95.3%,97.5%,95.2%,93.3%,91.1%,RSD分别为0.8%,0.7%,1.1%,0.9%,1.1%,1.0%,1.4%,1.0%（n=9）;方法检测限分别为15.37μg/g,0.86μg/g,0.38μg/g,8.30μg/g,0.090μg/g,1.59μg/g,1.27μg/g,0.12μg/g。结论该法快速、灵敏、准确、简便,色谱峰分离度良好,适用于硫辛酸原料药中有机残留溶剂的测定。
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, 3.0μm） 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, eyclohexane, 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 15.37μg/g, 0. 86 μg/g, 0.38 μg/g, 8.30 μg/g, 0. 090 μg/g, 1.59μg/g, 1.27μg/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 lipoie acid.
出处
《中国药业》
CAS
2016年第3期49-52,共4页
China Pharmaceuticals
