顶空毛细管气相色谱法测定琥珀酸舒马普坦中7种有机溶剂的残留量  

Determination of Residual Organic Solvents in Sumatriptan Succinate by Capillary Gas Chromatography with Headspace Sampling

作　　者：李娟[1] 蔡蓝洁[1] 艾朝辉[1] 孔杜林[1] 

机构地区：[1]海南医学院药学院,海南海口571199

出　　处：《广东化工》2015年第5期124-125,132,共3页Guangdong Chemical Industry

基　　金：海南省自然科学基金(813192)资助

摘　　要：目的：建立顶空毛细管气相色谱法,同时测定琥珀酸舒马普坦中甲醇、乙醇、丙酮、二氯甲烷、乙酸乙酯、四氢呋喃和环己烷七种溶剂残留量的方法。方法：采用DB-624毛细管气相色谱柱顶空进样法和FID检测器,同时测定琥珀酸舒马普坦中甲醇、乙醇、丙酮、二氯甲烷、乙酸乙酯、四氢呋喃和环己烷七种溶剂的残留量。结果：甲醇、乙醇、丙酮、二氯甲烷、乙酸乙酯、四氢呋喃和环己烷的线性范围分别为0.13~6.3mg·m L-1（r=0.9991）,0.16~7.9 mg·m L-1（r=0.9994）,0.16~7.9 mg·m L-1（r=0.9992）,0.03~1.3 mg·m L-1（r=0.9989）,0.18~9.0 mg·m L-1（r=0.9995）,0.02~0.9mg·m L-1（r=0.9988）,0.16~7.8 mg·m L-1（r=0.9992）;甲醇、乙醇、丙酮、二氯甲烷、乙酸乙酯、四氢呋喃和环己烷的平均回收率分别为102.4%、99.6%、98.8%、98.0%、100.4%、95.7%、96.5%（n=9）;RSD分别为1.8%、1.4%、2.5%、1.9%、1.6%、2.7%、1.8%（n=9）。结论：本方法简单、准确、灵敏度高、重现性好,能很好地测定琥珀酸舒马普坦中七种有机溶剂残留量的含量。Objective To develop headspace gas chromatography method for the determination of seven kinds of residual organic solvents in sumatriptan succinate.Methods The samples were injected into DB-624 capillary column by headspace sampler and analyzed with FID detector.Results The linear ranges of methanol,ethanol,acetone,dichloromethane,ethyl acetate,tetrahydro furan and cyclohexane were 0.13~6.3 mg·m L-1（r=0.9991）,0.16~7.9 mg·m L-1（r=0.9994）,0.16~7.9 mg·m L-1（r=0.9992）,0.03~1.3 mg·m L-1（r=0.9989）,0.18~9.0 mg·m L-1（r=0.9995）,0.02~0.9 mg·m L-1（r=0.9988）,0.16~7.8 mg·m L-1（r=0.9992）.The recoveries were 102.4 %、99.6 %、98.8 %、98.0 %、100.4 %、95.7 %、96.5 %（n=9）.The RSD were 1.8 %、1.4 %、2.5 %、1.9 %、1.6 %、2.7 %、1.8 %（n=9）respectively.Conclusion The method is simple,accurate and sensitive with good reproducibility.It can be used for the determination of the residual organic solvents in sumatriptan succinate.

关 键 词：毛细管气相色谱法 顶空进样法 琥珀酸舒马普坦 有机溶剂残留量 

分 类 号：O65[理学—分析化学]