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ZORBAX Eclipse Plus C18为色谱柱,乙腈-0.01 mol/L乙酸铵溶液(p H6.0)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(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 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 10μL.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 0.200-1.503μg/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 0.039μg/mL.The quantitation limits were 0.152,0.122,0.162,0.090,0.258,0.132,0.380,0.181,0.185 and 0.130μg/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 enterpriseⅠ,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 enterpriseⅡ,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.
作者
保敏敏
吕蓓蓓
魏文芝
张敏娟
BAO Minmin;LYU Beibei;WEI Wenzhi;ZHANG Minjuan(School of Medicine,Qinghai University,Xining 810016,China;Qinghai Provincial Drug Inspection and Testing Institute/Qinghai Provincial Key Laboratory of Modernization of Traditional Chinese and Tibetan Medicine/NMPA Key Laboratory for Quality Control of Traditional Chinese Medicine(Tibetan Medicine),Xining 810016,China)
出处
《中国药房》
CAS
北大核心
2023年第10期1199-1203,共5页
China Pharmacy
基金
国家药品抽检计划项目(No.国药监药管[2019]2号)。
作者简介
第一作者:保敏敏,硕士研究生。研究方向:药品质量控制与评价。Email:QH199809@163.com;通信作者:张敏娟,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。
