| 张伟,梁成罡.药品标准中杂质测定方法对国家标准物质赋值的影响[J].中国药品标准,2023,24(2): |
| 药品标准中杂质测定方法对国家标准物质赋值的影响 |
| Influence of impurity determination method in drug standard on national standard material assignment—Determination of free heptanic acid in norethisterone enanthate by gas chromatography |
| 投稿时间：2022-10-11 修订日期：2023-04-03 |
| DOI： |
| 中文关键词: 国家标准物质 赋值 气相色谱法 庚酸炔诺酮 游离庚酸 |
| 英文关键词: national drug standard assignment gas chromatography norethisterone enanthate free heptanic |
| 基金项目: |
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| 摘要点击次数: 32 |
| 全文下载次数: 23 |
| 中文摘要: |
| 目的：研究并建立气相色谱法(GC)法测定庚酸炔诺酮中游离庚酸的含量。方法：采用HP-FFAP(0.53mm×30m,1.00μm)毛细管色谱柱(固定相为硝基对苯二甲酸改性的聚乙二醇),以氮气为载气,FID检测器,采用程序升温,分流直接进样,标准曲线法计算游离庚酸的含量。结果：游离庚酸的检测限为0.49ng,定量限为2.45ng,线性范围9.84～118.04 μg.mL-1(r=0.999 9),平均回收率(n=3)为98.8%～101.0%(RSD=1.24%)。结论：本方法简单、快速、灵敏、准确,可对庚酸炔诺酮中游离庚酸进行质量控制。 |
| 英文摘要: |
| Objective: To research and establish a Gas Chromatography (GC) method for determination of free heptanic acid in norethisterone enanthate. Methods: free heptanic was determinated by GC with an HP-FFAP capillary column(0.53mm×30m,1.00μm). The carrier gas was nitrogen gas and FID was as detector. The injector and the detector temperature were both set at 240℃. the column temperature program was as follows: initial temperature was at 40℃, with the increase rate of 6℃.mL-1 to 230℃(hold 8 min). the free heptanic was calculated by standard curve method. Results: The detection limit for free heptanic was 0.49ng.mL-1, LOQ was 2.45ng.mL-1. The calibration curves showed good linearity in the range of 9.84～118.04μg.mL-1(r=0.999 9). The average recovery (n=3)of heptanic was 98.8%～101.0%(RSD=1.24%). Conclusions: This method is simple, fast, sensitive, accurate and suitable for the quality control of free heptanic in norethisterone enanthate. |
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