GC测定拉科酰胺原料药中的5种残留溶剂.PDFVIP

GC 测定拉科酰胺原料药中的 5 种残留溶剂  1 1 2* 胡剀 ，宋珊珊 ，王向军 (1.浙江九洲药业股份有限公司，浙江 台州 318000 ；2.浙江农林大学林业与生物技术学院，浙江 临安 311300) 摘要：目的 建立顶空进样气相色谱法检测拉科酰胺原料药中5 种残留溶剂的方法。方法 采用顶空毛细管气相色谱法， 色谱柱为Agilent HP-5 石英毛细管柱(30.0 m×0.32 mm×0.25 μm) ；进样口温度：210 ℃；FID 检测器温度：240 ℃；柱温： 1 50 ℃；载气：氮气；流速：1.0 mL·min 。顶空进样，顶空平衡温度：85 ℃，顶空平衡时间：30 min ；进样体积：0.35 mL 。 结果 在上述条件下，5 种残留溶剂均能良好分离，各溶剂峰面积与浓度均呈良好的线性关系，方法精密度良好，回收 率均较为理想。结论 该法适用于拉科酰胺原料药中残留溶剂的测定。 关键词：拉科酰胺；残留溶剂；顶空气相色谱法 中图分类号：R917.101 文献标志码：B 文章编号：1007-7693(2014)03-0343-03 Determination of Five Residual Organic Solvents in Lacosamide by GC 1 1 2* HU Kai , SONG Shanshan , WANG Xiangjun (1.Zhejiang Jiuzhou Pharmaceutical Co., Ltd, Taizhou 318000, China; 2.School of Forestry and Bio-technology, Zhejiang AF University, Lin’an 311300, China) ABSTRACT: OBJECTIVE To establish a headspace gas chromatography method for determination of residual solvents in lacosamide. METHODS Headspace gas chromatography was added using an Agilent HP-5 capillary column(30.0 m× 0.32 mm×0.25 μm). The column temperature was 50 ℃with nitrogen gas as carrier and FID as detector. The flow of carrier was −1 1.0 mL·min . The injection port and detector temperature were 210 ℃and 240 ℃ , respectively. The heated temperature of the headspace oven was 85 ℃ , the heated time lasted 30 min, and the injection volume was 0.35 mL. RESULTS Each solvent could be completely separated in chromatogram obtained from systemic suitability test, and the calibration curves of each solvent had good linear relationship within a certain range. CONCLUSION The method is accurate and reliable. It can be applied in determination of residual solvents in lacosamide. KEY WORDS: lacosamide; residual so