| 引用本文: | 孙红,赵龙山,陈素娥.依帕司他原料药有关物质的HPLC测定方法改进研究[J].中国现代应用药学,2019,36(16):2057-2061. |
| SUN Hong,ZHAO Longshan,CHEN Su'e.Improvement Research of Determination for the Related Substances in Epalrestat by HPLC[J].Chin J Mod Appl Pharm(中国现代应用药学),2019,36(16):2057-2061. |
|
| 摘要: |
| 目的 采用改进的高效液相色谱法测定依帕司他原料药有关物质。方法 采用依利特Hypersil BDS C18色谱柱（250 mm×4.6 mm，5 μm），以乙腈-pH6.5磷酸盐缓冲液（0.025 mol·L-1 KH2PO4+0.025 mol·L-1 Na2HPO4，用H3PO4调节pH至6.5）为流动相，梯度洗脱，流速为1.0 mL·min-1，检测波长为396 nm和280 nm，柱温为30℃，进样量为20 μL。结果 依帕司他与相邻杂质能较好地分离。立体异构体杂质在浓度0.010~30 μg·mL-1内线性关系良好，检测限和定量限分别为0.80，2.4 ng·mL-1。精密度、稳定性、准确度、耐用性均符合要求。结论 该方法可用于依帕司他原料药有关物质的检查。 |
| 关键词: 依帕司他 有关物质 立体异构体 未知杂质 高效液相色谱法 |
| DOI：10.13748/j.cnki.issn1007-7693.2019.16.015 |
| 分类号:R917.101 |
| 基金项目: |
|
| Improvement Research of Determination for the Related Substances in Epalrestat by HPLC |
|
SUN Hong1, ZHAO Longshan2, CHEN Su'e1
|
|
1.Shanxi Health Vacational College, Jinzhong 030619, China;2.Shenyang Pharmaceutical University, Shenyang 110013, China
|
| Abstract: |
| OBJECTIVE To establish an improved HPLC method for the determination of the related substances in epalrestat. METHODS The chromatographic seperation was achieved on an Elite Hypersil BDS C18 column(250 mm×4.6 mm, 5 μm) with the mobile phase consisted of acetonitrile-phosphate buffer salt (0.025 mol·L-1 KH2PO4 + 0.025 mol·L-1 Na2HPO4) at pH 6.5 adjusted with phosphoric acid, used gradient elution at the flow rate of 1.0 mL·min-1. The detection wavelengths were set at 396 nm and 280 nm, and the injection volume was 20 μL. The column temperature was maintained at 30℃. RESULTS The stereoisomer had good linear relationship within the range of concentration of 0.010-30 μg·mL-1, the LOD and LOQ of stereoisomer was 0.80 and 2.4 ng·mL-1, respectively. Other validation parameters, including precision, sample stability, accuracy and robustness were all within the acceptance range. CONCLUSION The developed method is successfully applied to the determination of related substances in epalrestat. |
| Key words: epalrestat related substances stereoisomer unknown impurities HPLC |
