| 黄美容,曹阳,黄顺旺,等.高效液相色谱法测定盐酸伐地那非原料药中的有关物质[J].安徽医药,2021,25(7):1290-1294. |
| 高效液相色谱法测定盐酸伐地那非原料药中的有关物质 |
| Determination of related substances in Vardenafil hydrochloride by HPLC |
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| DOI：10.3969/j.issn.1009-6469.2021.07.005 |
| 中文关键词: 伐地那非 色谱法，高压液相 药物污染 主成分分析 |
| 英文关键词: Vardenafil Chromatography, high pressure liquid Drug contamination Principal component analysis |
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| 中文摘要: |
| 目的建立高效液相色谱法( HPLC)测定盐酸伐地那非中的有关物质。方法采用反相 HPLC，色谱柱为 Agilent HCC18(2)流动相 A为 0.5%三乙胺溶液(用磷酸调节 pH至 3.0)-乙腈( 90∶10)，流动相 B为 0.5%三乙胺溶液(用磷酸调节 pH至 3.0) (10∶90)梯度洗脱，检测波长 242 nm，以外标法计算已知杂质的含量，主成分自身对照法计算未知杂质的含量。结-乙腈，果盐酸伐地那非和，杂质 A、B、C、D、E、F、G7个已知杂质的分离度均符合要求( ≥1.5)；盐酸伐地那非与 7个杂质的浓度与峰面积呈良好的线性关系，相关系数均在 0.998以上；杂质 A、B、C、D、E、F、G杂质的平均回收率分别为 99.8%、101.6%、102.4%、99.5%、100.5%、101.7%、103.6%，在 99.5% ~ 103.6%范围内， RSD分别为 1.8%、0.6%、1.2%、1.4%、0.9%、1.5%、0.9%，均<2%。结论该方法准确、灵敏、精密度良好，可定量分析 7个工艺杂质和降解杂质，可作为盐酸伐地那非原料有关物质的检测方法。 |
| 英文摘要: |
| Objective To establish HPLC method for the determination of the related substances in Vardenafil hydrochloride.Meth? ods An RP-HPLC method was used,the column was Agilent HC-C18 (2), the mobile phase A was 0.5% triethylamine solution (adjusted to pH 3.0with phosphoric acid)-acetonitrile(90:10), themobile phaseB was 0.5% triethylamine solution (adjusted to pH 3.0withphosphoric acid)-acetonitrile(10:90), gradient elution, detection wavelength 242 nm. The content of known impurities was calculated by externalstandard method, and the content of unknown impurities was calculated by principal component self-control method.Results The separation of Vardenafilhydrochloride and seven known impurities A,B,C, D,E,F and G allmet the requirements (≥ 1.5); there was a good linearrelationship between the concentration and peak area of vardenafil hydrochloride and seven impurities, and the correlation coefficientswere all above 0.998; The average recoveries of impurities A, B, C, D,E, F and G were 99.8%, 101.6%, 102.4%, 99.5%, 100.5%, 101.7%and 103.6%, respectively. Within the range of 99.5% -103.6%, RSD were 1.8%, 0.6%, 1.2%, 1.4%, 0.9%, 1.5% and 0.9%, respectively, all less than 2%.Conclusion The method is accurate, sensitive and precise. It can be used for the quantitative analysis of seven processimpuritiesand degradationimpurities.Itcanbeusedforthedeterminationofrelatedsubstancesin vardenafilhydrochloride. |
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