郭拥政,孙晓群,陈程,唐郑勇,章海燕,鲍淳昊.HPLC法测定缬沙坦中的遗传毒性杂质[J].中国药品标准,2016,17(5):337-340 |
HPLC法测定缬沙坦中的遗传毒性杂质 |
HPLC Determination of Genotoxic Impurities in Valsartan |
投稿时间:2016-04-28 修订日期:2016-08-18 |
DOI: |
中文关键词: 高效液相色谱 缬沙坦 遗传毒性杂质 |
英文关键词: HPLC Valsartan genotoxic impurity |
基金项目: |
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中文摘要: |
目的:建立缬沙坦中潜在的遗传毒性杂质2-氰基-4'-溴甲基联苯(杂质1)和2-氰基-4',4'-二溴甲基联苯(杂质2)的含量测定方法。方法:采用高效液相色谱法,色谱柱为C18 (4.6 mm×250 mm,5 μm),流动相为乙腈-水-冰乙酸(700:300:1),检测波长210nm,流量0.8 mL?min-1,柱温30 ℃,进样量20 μL。结果:杂质1和杂质2与主成分之间分离度良好,在0.045-~0.18 μg?mL-1的浓度范围内杂质1和杂质2的峰面积呈良好的线性关系( 相关系数分别为1.000和0.999 5);杂质1和杂质2的平均回收率分别为96.57%和107.38%,RSD(n=9)分别为1.9%和7%。结论:所建方法简单、准确、重复性好,适用于缬沙坦中的遗传毒性杂质检测。 |
英文摘要: |
Objective: To establish an HPLC method for the determination of potential genotoxic impurities : 2-cyano-4′-bromomethyl biphenyl (impurity 1) and 2-cyano-4,4′-bisbromomethyl biphenyl (impurity 2) in Valsartan. Methods: The separation was performed on a C18 column (4.6mm×250 mm, 5μm) with the mobile phase of acetonitrile- water - glacial acetic acid (700 : 300 : 1) at a flow rate of 0.8 mL?min-1, the injection volume was 20 μL with the detection wavelength at 210 nm, the column temperature was 30 oC. Results: Impurity 1and impurity 2 could be well separated from Valsartan, and the calibration curve for impurity 1 and impurity 2 were linear in the range of 0.045–0.18 μg?mL -1(r1=1.000, r2=0.999 5). Furthermore, the average recovery for impurity 1 and impurity 2 was 96.57% and 107.38% with RSD(n=9) of 1.9% and 7%, respectively. Conclusion:The method is simple, accurateand repeatable, which is suitable for the detection of genotoxic impurities in Valsartan. |
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