| 引用本文: | 张巍,蔡犇,李范珠.顶空气相色谱法测定依帕司他有机溶剂残留量[J].中国现代应用药学,2017,34(9):1286-1288. |
| ZHANG Wei,CAI Ben,LI Fanzhu.Determination of Residual Organic Solvents in Epalrestat by Headspace GC[J].Chin J Mod Appl Pharm(中国现代应用药学),2017,34(9):1286-1288. |
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| 摘要: |
| 目的 建立测定依帕司他原料药中残留有机溶剂甲醇、乙醇、二氯甲烷、正己烷、乙酸乙酯、四氢呋喃、甲苯的检测方法，为建立质量标准提供依据。方法 采用DB-624毛细管柱（30 m×0.53 mm，3.0 μm），氢火焰离子化检测器（FID），进样口温度210℃，检测器温度250℃，程序升温，流速3.0 mL·min-1，分流比10：1，顶空平衡温度85℃，平衡时间30 min，按内标法（内标物叔戊醇）测定各残留溶剂的含量。结果 药物中7种残留溶剂的精密度RSD均<5%，在各自的浓度范围内具有良好的线性关系，相关系数均>0.999，平均回收率为90.0%~100.0%。结论 本方法专属性好，灵敏度高，操作简单，测定结果准确，适用于依帕司他原料药7种残留溶剂的同时测定。 |
| 关键词: 依帕司他 残留溶剂 顶空气相色谱法 |
| DOI：10.13748/j.cnki.issn1007-7693.2017.09.015 |
| 分类号:R917.101 |
| 基金项目: |
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| Determination of Residual Organic Solvents in Epalrestat by Headspace GC |
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ZHANG Wei1,2, CAI Ben2, LI Fanzhu1
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1.Zhejiang Chinese Medical University, Hangzhou 310053, China;2.Zhejiang Yongning Pharmaceutical Co., Ltd., Taizhou 318020, China
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| Abstract: |
| OBJECTIVE To establish a method for the determination of residual solvents (methanol, ethanol, dichloromethane, n-hexane, ethyl acetate, tetrahydrofuran, toluene) in epalrestat for controlling the quality of epalrestat. METHODS The solvents were separated on DB-624 capillary column(30 m×0.53 mm, 3.0 μm) with programming temperature, and detected using hydrogen flame ionization detector(FID). The headspace and other chromatographic conditions were as follows:250℃ of detector temperature, 3.0 mL·min-1 of flow rate, 10:1 of split ratio, 210℃ of inlet temperature, 85℃ of equilibrium temperature and 30 min of equilibrium time. The contents of residual solvents were determined according to the internal standard method(internal standard tert-amyl alcohol). RESULTS There were good linear relationship in the concentration ranges with correlation coefficient above 0.999, respectively. The precisions (RSD values) were less than 5% in all seven kinds of residual solvents, and the average recoveries were within 90.0%-100.0%. CONCLUSION This method had good specificity, high sensitivity, simple operation and accurate results. It was suitable for the determination of above 7 kinds of residual solvents in Epalrestat API at same time. |
| Key words: epalrestat residual solvent headspace GC |
