| 引用本文: | 李丹凤,朱健萍,卢日刚.GC测定甘氨酸原料药中12种有机溶剂的残留量[J].中国现代应用药学,2018,35(11):1637-1641. |
| LI Danfeng,ZHU Jianping,LU Rigang.Determination of 12 Residual Organic Solvents in the Raw Material of Glycine by GC[J].Chin J Mod Appl Pharm(中国现代应用药学),2018,35(11):1637-1641. |
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| 摘要: |
| 目的 建立同时测定甘氨酸原料药中甲醇、乙醇、丙酮、异丙醇、乙腈、二氯甲烷、正丙醇、乙酸乙酯、四氢呋喃、环己烷、正丁醇和甲苯12种有机溶剂残留量的方法。方法 采用DB-624毛细管柱（30 m×0.53 mm，3.0 μm）程序升温，氢火焰离子化检测器（FID），进样口温度为150℃，检测器温度为250℃，载气为高纯氮气，载气流速为2.2 mL·min-1，分流比为10∶1，顶空加热温度为80℃，平衡时间为35 min。结果 甘氨酸中12种残留溶剂在各自质量浓度范围内与峰面积线性关系良好（r均>0.999）；精密度、稳定性试验的RSD均<5%，重复性试验中只检出乙醇、丙酮、异丙醇（RSD≤1.8%）；平均加样回收率为97%~102%。结论 该方法操作简单、快速灵敏、结果准确，可用于甘氨酸原料药中12种有机溶剂残留量测定。 |
| 关键词: 甘氨酸 原料药 残留溶剂 气相色谱法 |
| DOI：10.13748/j.cnki.issn1007-7693.2018.11.009 |
| 分类号:R917 |
| 基金项目: |
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| Determination of 12 Residual Organic Solvents in the Raw Material of Glycine by GC |
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LI Danfeng, ZHU Jianping, LU Rigang
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Guangxi Zhuang Autonomous Region Institute for Food and Drug Control, Nanning 530021, China
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| Abstract: |
| OBJECTIVE To establish a method for the determination of 12 residual organic solvents in glycine as methanol, alcohol, acetone, isopropyl alcohol, acetonitrile, dichloromethane, N-propanol, ethyl acetate, tetrahydrofuran, cyclohexane, N-butyl alcohol, and toluene. METHODS Headspace GC was adopted. The determination was performed on DB-624 capillary column (30 m×0.53 mm, 3.0 μm) using temperature programming with FID. The inlet temperature was 150℃, and flame ionization detector was used with temperature of 250℃. High purity nitrogen was used as carrier gas with flow rate of 2.2 mL·min-1. The split ratio was 10:1. Headspace heating temperature was 80℃, and equilibration time was 35 min. RESULTS There was good linear relationship in the concentration ranges of 12 residual organic solvents with correlation coefficient above 0.999, respectively. RSDs of precision and stability tests were all <5%, and alcohol, acetone and isopropyl alcohol were found in repeatability test (RSD ≤ 1.8%). The average recoveries were within 97%-102%. CONCLUSION The established method is simple, accurate and reproducible, and can be used for simultaneous determination of 12 residual organic solvents in the raw material of glycine. |
| Key words: glycine raw material residual solvents GC |
