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奥卡西平片中有关物质含量测定方法的建立
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| 篇名： | 奥卡西平片中有关物质含量测定方法的建立 |
| TITLE： | Method establishment for content determination of related substances in Oxcarbazepine tablets |
| 摘要： | 目的 建立奥卡西平片中有关物质的含量测定方法。方法采用超高效液相色谱（UPLC）法，以ZORBAXEclipsePlusC18为色谱柱，乙腈-0.01mol/L乙酸铵溶液（pH6.0）为流动相进行梯度洗脱，流速为0.5mL/min，检测波长为230nm，柱温为35℃，进样量为10μL。结果奥卡西平和杂质A、B、C、D、E、I、K、L、N检测质量浓度线性范围分别为0.192～1.440、1.019～7.639、0.208～1.559、0.230～1.727、0.389～2.915、0.182～1.364、0.393～2.945、0.199～1.493、0.199～1.490、0.200～1.503μg/mL（r均大于0.999）；检测限分别为0.046、0.037、0.049、0.027、0.077、0.040、0.114、0.054、0.055、0.039μg/mL，定量限分别为0.152、0.122、0.162、0.090、0.258、0.132、0.380、0.181、0.185、0.130μg/mL；精密度、重复性、稳定性（24h）、耐用性试验的RSD均小于5.0%；平均回收率为92.8%～105.6%（RSD≤3.0%，n＝9）。原研制剂样品中仅检出杂质K和未知杂质，其总含量为0.078%～0.083%；国内Ⅰ企业产仿制制剂样品中检出杂质A、B、D、I和未知杂质，其总含量为0.147%～0.163%；国内Ⅱ企业产仿制制剂样品中检出杂质A、B、I和未知杂质，其总含量为0.085%～0.161%。结论所建UPLC法快速，灵敏度高，准确度、稳定性、耐用性好，可用于同时测定奥卡西平片中9种已知杂质的含量。 |
| ABSTRACT： | OBJECTIVE To establish the method for content determination of related substances in Oxcarbazepine tablets. METHODS Ultra-high performance liquid chromatography （UPLC） method was adopted and the separation was performed on ZORBAX Eclipse Plus C18 column with mobile phase consisted of acetonitrile-0.01 mol/L ammonium acetate solution （pH6.0） （gradient elution） at the flow rate of 0.5 mL/min. The detection wavelength was 230 nm and column temperature was set at 35 ℃. The sample size was 10 μL. RESULTS The linear ranges of oxcarbazepine and impurity A， B， C， D， E， I， K， L and N were 0.192-1.440， 1.019-7.639， 0.208-1.559， 0.230-1.727， 0.389-2.915， 0.182-1.364， 0.393-2.945， 0.199-1.493， 0.199-1.490 and 0.200- 1.503 μg/mL， respectively （all r＞0.999）. The detection limits were 0.046， 0.037， 0.049， 0.027， 0.077， 0.040， 0.114， 0.054， 0.055 and 0.039 μg/mL. The quantitation limits were 0.152， 0.122， 0.162， 0.090， 0.258， 0.132， 0.380， 0.181， 0.185 and 0.130 μg/mL. RSDs of precision， repeatability， stability （24 h） and durability tests were all lower than 5.0%. The average recoveries were 92.8%-105.6% （RSD≤3.0%， n＝9）. Only impurity K and unknown impurity were detected in the original preparation sample， with a total content of 0.078% to 0.083%； impurities A， B， D， I and unknown impurity were detected in the generic preparations produced by domestic enterprise Ⅰ， with a total content of 0.147% to 0.163%； impurities A， B， I and unknown impurity were detected in the generic preparations produced by domestic enterprise Ⅱ， with a total content of 0.085% to 0.161%. CONCLUSIONS The established method is rapid， sensitive， accurate， stable and durable. It can be used for the content determination of 9 known impurities in Oxcarbazepine tablets. |
| 期刊： | 2023年第34卷第10期 |
| 作者： | 保敏敏；吕蓓蓓；魏文芝；张敏娟 |
| AUTHORS： | BAO Minmin，LYU Beibei，WEI Wenzhi，ZHANG Minjuan |
| 关键字： | 奥卡西平片；超高效液相色谱法；有关物质；含量测定 |
| KEYWORDS： | Oxcarbazepine tablets； UPLC； related substance； content determination |
| 阅读数： | 87 次 |
| 本月下载数： | 2 次 |
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