| 摘要: |
| 目的 建立HPLC测定异维A酸有关物质的方法。方法 色谱柱为NUCLEOSIL 100-3 C18（4.6 mm×150 mm，3 μm），以甲醇-水-冰醋酸（770：225：5）为流动相，流速为1.0 mL·min-1；柱温为25℃，检测波长为355 nm。结果 异维A酸峰与杂质H、I、维A酸、强制降解杂质峰分离良好；异维A酸、杂质H、I和维A酸的线性范围分别为0.000 545 5~21.82 μg·mL-1（r=0.999 9），0.002 856~7.14 μg·mL-1（r=0.999 0），0.002 789~6.97 μg·mL-1（r=0.999 1）、0.017 07~22.76 μg·mL-1（r=0.999 6）；检测限分别为0.27，0.60，0.65，5.50 ng·mL-1，定量限分别为0.55，2.85，2.80，17.00 ng·mL-1；杂质H、I和维A酸的平均回收率分别为101.57%，102.02%，101.03%，RSD分别为0.5%，0.8%，1.5%。结论 建立的HPLC方法准确、专属性强，可用于异维A酸有关物质的测定。 |
| 关键词: 异维A酸 有关物质 高效液相色谱法 |
| DOI：10.13748/j.cnki.issn1007-7693.2019.01.009 |
| 分类号:R917.101 |
| 基金项目:国家药典委员会国家药品标准提高研究项目（食药监办药化管[2016]141号） |
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| Determination of Related Substances of Isotretinoin by HPLC |
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TANG Yang
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Chongqing Institute for Food and Drug Control, Chongqing Engineering Research Center for Pharmaceutical Process and Quality Control, Chongqing 401121, China
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| Abstract: |
| OBJECTIVE To develop a method for related substances determination of isotretinoin by HPLC. METHODS NUCLEOSIL 100-3 C18 column (4.6 mm×150 mm, 3 μm) was used. The mobile phase was consisted of methanol-water-glacial acetic acid(770:225:5) with a flow rate of 1.0 mL·min-1. The column temperature was 25℃, and detection wavelength was 355 nm. RESULTS Chromatographic peaks of isotretinoin and impurity H, I, tretinoin, degradation impurities were separated. Linear ranges of isotretinoin, impurity H, I and tretinoin were 0.000 545 5-21.82 μg·mL-1(r=0.999 9), 0.002 856-7.14 μg·mL-1 (r=0.999 0), 0.002 789-6.97 μg·mL-1(r=0.999 1), 0.017 07-22.76 μg·mL-1(r=0.999 6), respectively; LODs were 0.27, 0.60, 0.65, 5.50 ng·mL-1; LOQs were 0.55, 2.85, 2.80, 17.00 ng·mL-1. Average recoveries of impurity H, I and tretinoin were 101.57%, 102.02%, 101.03%, and RSDs were 0.5%, 0.8%, 1.5%. CONCLUSION The HPLC method is accurate, specific and reliable for determination of related substances of isotretinoin. |
| Key words: isotretinoin related substances HPLC |
