| 于风平,闫敏,舒希凯,邱增英,贺敦伟.反向离子对色谱法测定格列吡嗪原料药中5-甲基-2-吡嗪羧酸的含量[J].中国药品标准,2018,19(6):482-487 |
| 反向离子对色谱法测定格列吡嗪原料药中5-甲基-2-吡嗪羧酸的含量 |
| Determination of 5-methyl-2-pyrazine carboxylic acid in glipizide by reverse ion pair chromatography |
| 投稿时间：2018-09-30 修订日期：2018-11-30 |
| DOI： |
| 中文关键词: 格列吡嗪 HPLC 离子对色谱 5-甲基-2-吡嗪羧酸 方法验证 |
| 英文关键词: glipizide HPLC ion pair chromatography 5- methyl -2- pyrazine carboxylic acid method verification |
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| 中文摘要: |
| 目的：建立格列吡嗪原料药中5-甲基-2-吡嗪羧酸的含量测定方法。方法：采用反向离子对色谱法。色谱柱为Agilent Eclipse XDB-C18，流动相：50 mmol?L-1NaH2PO4溶液（含0.05%四丁基氢氧化铵）-甲醇（梯度洗脱），流速为1.0 mL?min-1，柱温为30 ℃，检测波长为276 nm，进样量为20μL。结果：5-甲基-2-吡嗪羧酸质量浓度线性范围为0.0385~1.4453μg?mL-1（r＝0.9999，n＝5），检测限为0.01155μg?mL-1，定量限为0.0385μg?mL-1；平均回收率为100.94%，RSD为1.4%（n=9）；系统精密度、重复性、中间精密度试验结果良好；对照品和供试品溶液8h稳定；3批原料药中5-甲基-2-吡嗪羧酸的量分别为0.0083%、0.0085%、0.0092%。结论：本方法操作简便、方法灵敏、结果准确可靠，可用于格列吡嗪原料药中微量杂质5-甲基-2-吡嗪羧酸的测定。 |
| 英文摘要: |
| ABSTRACT Objective: To establish a method for the determination of 5- methyl -2- pyrazine carboxylic acid in glipizide. Methods: Reverse ion pair chromatography was used. The chromatographic column was Agilent Eclipse XDB-C18 with a mobile phase of 50 mmol/L NaH2PO4 solution (containing 0.05% tetrabutylammonium hydroxide) -methanol (gradient elution), a flow rate of 1.0 mL/min, a column temperature of 30 C, a detection wavelength of 276 nm, and a sample size of 20 uL. Results: The linear range of 5-methyl-2-pyrazine carboxylic acid was 0.0385~1.4453 ug/ml (r=0.9999, n=5), the detection limit was 0.01155 ug/ml, the quantitative limit was 0.0385 ug/ml.The average recovery was 100.94%, RSD was 1.4% (n=9).The system precision, repeatability and intermediate precision test results were good.The control and test samples were stable for 8 hours. The amount of 5- methyl -2- pyrazine carboxylic acid in the 3 batch of API was 0.0083%,0.0085% and 0.0092%. Conclusion: The method is simple, sensitive, accurate and reliable, and can be used for the determination of 5-methyl-2-pyrazine carboxylic acid in glipizide. |
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