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1.青海大学医学院,西宁;810016
2.青海省药品检验检测院/青海省中藏药现代化研究重点实验室/国家药品监督管理局中药(藏药)质量控制重点实验室,西宁 810016
硕士研究生。研究方向:药品质量控制与评价。E-mail:QH199809@163.com
主任药师,硕士生导师。研究方向:药品质量分析、药品质量标准。电话:0971-8247794。E-mail:1415328549@qq.com
纸质出版日期:2023-05-30,
收稿日期:2022-10-30,
修回日期:2023-03-26,
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保敏敏,吕蓓蓓,魏文芝等.奥卡西平片中有关物质含量测定方法的建立 Δ[J].中国药房,2023,34(10):1199-1203.
BAO Minmin,LYU Beibei,WEI Wenzhi,et al.Method establishment for content determination of related substances in Oxcarbazepine tablets[J].ZHONGGUO YAOFANG,2023,34(10):1199-1203.
保敏敏,吕蓓蓓,魏文芝等.奥卡西平片中有关物质含量测定方法的建立 Δ[J].中国药房,2023,34(10):1199-1203. DOI: 10.6039/j.issn.1001-0408.2023.10.09.
BAO Minmin,LYU Beibei,WEI Wenzhi,et al.Method establishment for content determination of related substances in Oxcarbazepine tablets[J].ZHONGGUO YAOFANG,2023,34(10):1199-1203. DOI: 10.6039/j.issn.1001-0408.2023.10.09.
目的
2
建立奥卡西平片中有关物质的含量测定方法。
方法
2
采用超高效液相色谱(UPLC)法,以ZORBAX Eclipse Plus C
18
为色谱柱,乙腈-0.01 mol/L乙酸铵溶液(pH6.0)为流动相进行梯度洗脱,流速为0.5 mL/min,检测波长为230 nm,柱温为35 ℃,进样量为10 μL。
结果
2
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、0.200~1.503 μg/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、0.039 μg/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、0.130 μg/mL;精密度、重复性、稳定性(24 h)、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
2
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。
OBJECTIVE
2
To establish the method for content determination of related substances in Oxcarbazepine tablets.
METHODS
2
Ultra-high performance liquid chromatography (UPLC) method was adopted and the separation was performed on ZORBAX Eclipse Plus C
18
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
2
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
2
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.
奥卡西平片超高效液相色谱法有关物质含量测定
UPLCrelated substancecontent determination
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VELUGULA S R K,REDDY A S K,MISRA N C,et al. Synthesis and characterization of potential impurities of oxcarbazepine drug substance:an antiepileptic agent[J]. J Heterocycl Chem,2021,58(8):1581-1587.
FAUDONE S N,PASCHOAL A R,CARVALHO P S, Jr,et al. X-ray diffraction,vibrational and thermal study of dibenzazepinodione,a pharmacopeial impurity of oxcarbazepine[J]. J Mol Struct,2019,1182:204-212.
SUN Y H,LI M,HADIZADEH M H,et al. Theoretical insights into the degradation mechanisms,kinetics and eco-toxicity of oxcarbazepine initiated by OH radicals in aqueous environments[J]. J Environ Sci(China),2023,129:189-201.
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