| 戴学东,董莉.GC柱前衍生化法测定盐酸二甲双胍和0.5%硬脂酸镁中硬脂酸镁的含量[J].中国药事,2017,(5):555-559 |
| GC柱前衍生化法测定盐酸二甲双胍和0.5%硬脂酸镁中硬脂酸镁的含量 |
| Determination of the Content of Magnesium in Metformin Hydrochloride and 0.5% Magnesium Stearate by Pre-column Derivatization GC Method |
| 投稿时间：2016-11-14 |
| DOI：10.16153/j.1002-7777.2017.05.016 |
| 中文关键词: GC 柱前衍生化 盐酸二甲双胍 硬脂酸镁 含量测定 |
| 英文关键词: GC pre-column derivatization metformin hydrochloride magnesium stearate content determination |
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| 中文摘要: |
| 目的：建立柱前衍生化气相色谱法测定盐酸二甲双胍+0.5%硬脂酸镁中硬脂酸镁的含量。方法：以12%三氟化硼甲醇溶液作为衍生化试剂，在50 ℃水浴振荡器中加热15 min的反应条件，采用不饱和脂肪酸甲酯化方法，使其生成棕榈酸甲酯和硬脂酸甲酯，以菲作为内标，用TG-WAXMS石英毛细管柱（聚乙二醇-20M为固定液），起始温度为190 ℃，以4 ℃·min-1的升温速率升温至220 ℃，维持15 min，进样口温度250 ℃，FID为检测器，检测器温度250 ℃。结果：硬脂酸镁浓度在0.125~1.00 mg·mL-1与峰面积呈良好的线性关系，平均回收率为100.01%，RSD为0.45%。结论：本方法灵敏、准确、可靠，可用于对原料药中加入的极少量硬脂酸镁进行质量控制。 |
| 英文摘要: |
| Objective: To establish a pre-column derivatization GC method for the determination of content of magnesium in metformin hydrochloride and 0.5% magnesium stearate. Methods: Unsaturated fatty acid methylester method was used to generate methyl palmitic acid and stearic acid methylester with 12% boron trifluoride methanol solution as derivative reagent, and heated to 50℃ with water bath shake for 15 minutes. Phenanthrene was used as internal standard. The determination was conducted by TG-WAXMS silica capillary column mixed with polyethylene glycol-20M as stationary liquid. The initial temperature was 190 ℃; and then it was raised to 220 ℃ at the rate of 4 ℃·min-1 and maintained for 15 minutes. Both the inlet and FID detector temperature were 250 ℃. Results: The magnesium stearate showed a good liner relationship with the peak area in the range of 0.125-1.00 mg·mL-1. The average recovery was 100.01%, RSD was 0.45%. Conclusion: The method is sensitive, accurate, reliable and suitable for quality control of tiny amounts of magnesium stearate in active ingredients. |
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