| 赵静芝,宿亮,朱婧,朱跃芳,吴超男.超高效液相色谱法测定富马酸伏诺拉生原料有关物质[J].中国药事,2022,36(7):800-809 |
| 超高效液相色谱法测定富马酸伏诺拉生原料有关物质 |
| Determination of the Related Substances in Vonoprazan Fumarate by Ultra High Performance Liquid Chromatography (UPLC) |
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| DOI：10.16153/j.1002-7777.2022.07.009 |
| 中文关键词: 消化性溃疡 富马酸伏诺拉生 有关物质 超高效液相色谱法 质量控制 |
| 英文关键词: peptic ulcer vonoprazan fumarate related substances ultra high performance liquid chromatography quality control |
| 基金项目:湖南省自然科学基金资助项目(编号 2017JJ2123) |
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| 中文摘要: |
| 目的：建立超高效液相色谱法测定富马酸伏诺拉生有关物质的方法。方法：采用ZORBAX SB-C18色谱柱(4.6 mm×150 mm，1.8 μm)，流动相A为0.025 mol·L-1磷酸盐缓冲溶液(pH 6.0)- 甲醇-乙腈(14∶5∶1)，流动相B为0.025 mol·L-1磷酸盐缓冲溶液(pH 6.0)-乙腈(3∶7)， 采用梯度洗脱，流速1.0 mL·min-1，柱温30 ℃，检测波长230 nm，进样量20 μL。结果：杂质A、 杂质C、杂质D、杂质F、杂质G、杂质H、杂质J、杂质K、杂质L、杂质M、杂质N和伏诺拉生分别在0.04177~2.088 μg·mL-1(r=1.0000)、0.07479~3.740 μg·mL-1(r=1.0000)、0.07335~3.668 μg·mL-1(r=1.0000)、0.1000~2.004 μg·mL-1(r=1.0000)、0.1325~6.623 μg·mL-1(r=1.0000)、 0.09300~1.860 μg·mL-1(r=1.0000)、0.1380~2.7530 μg·mL-1(r=1.0000)、0.1350~2.698 μg·mL-1 (r=1.0000)、0.1130~2.257 μg·mL-1(r=1.0000)、0.05060~2.530 μg·mL-1(r=0.9999)、 0.1420~2.846 μg·mL-1(r=1.0000)、0.1190~2.382 μg·mL-1(r=0.9998)浓度范围内与峰面积呈良好线性关系。上述各杂质的平均回收率(n=9)分别为97.24%、102.12%、99.46%、98.29%、101.51%、 100.84%、99.18%、101.20%、98.49%、103.63%、96.49%。采用该检测方法对5批样品进行有关物质检测，其中杂质C、杂质M、杂质N检出量均≤0.05%，杂质H、其他最大单个杂质检出量均≤0.10%，总杂质检出量均≤0.31%。结论：经方法学验证，本法专属性强、灵敏度高、准确度高，可用于富马酸伏诺拉生原料的有关物质测定，为其质量控制提供方法保证。 |
| 英文摘要: |
| Objective: To establish a method for the determination of related substances in vonoprazan fumarate by ultra high performance liquid chromatography (UPLC). Methods: ZORBAX SB-C18 column (4.6 mm×150 mm, 1.8 μm) was performed, the mobile phase A was 0.025 mol·L-1 phosphate buffer solution (pH 6.0)-methanol-acetonitrile (14∶5∶1), and the mobile phase B was 0.025 mol·L-1 phosphate buff er solution (pH 6.0)-acetonitrile (3∶7). Gradient elution was used, the fl ow rate was 1.0 mL·min-1, the column temperature was 30 ℃, the detection wavelength was 230 nm, and the injection volume was 20 μL. Results: Impurity A, impurity C, impurity D, impurity F, impurity G, impurity H, impurity J, impurity K, impurity L, impurity M, impurity N and vonoprazan in the concentration ranges of 0.04177-2.088 μg·mL-1 (r=1.0000), 0.07479-3.740 μg·mL-1 (r=1.0000), 0.07335-3.668 μg·mL-1 (r=1.0000), 0.1000-2.004 μg·mL-1 (r=1.0000), 0.1325-6.623 μg·mL-1 (r=1.0000), 0.09300-1.860 μg·mL-1 (r=1.0000), 0.1380-2.7530 μg·mL-1 (r=1.0000), 0.1350-2.698 μg·mL-1 (r=1.0000), 0.1130-2.257 μg·mL-1 (r=1.0000), 0.05060-2.530 μg·mL-1 (r=0.9999), 0.1420-2.846 μg·mL-1 (r=1.0000), and 0.1190-2.382 μg·mL-1 (r=0.9998) revealed good linear relationship with the peak area. The rates of recovery (n=9) of the above impurities were 97.24%, 102.12%, 99.46%, 98.29%, 101.51%, 100.84%, 99.18%, 101.20%, 98.49%, 103.63%, and 96.49% , respectively. Five batches of samples were tested for related substances by this detection method, in which the detection amount of impurity C, impurity m and impurity N was ≤ 0.05%, the detection amount of impurity h and other largest single impurities was ≤ 0.10%, and the total detection amount of impurities was ≤ 0.31%. Conclusion: The method has been proved to be exclusive, sensitive and accurate. It can be used to determine the related substances in vonoprazan fumarate materials and can provide a method guarantee for its quality control. |
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