高效液相色谱法同时测定盐酸多奈哌齐原料的十种有关物质
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摘要
目的建立高效液相色谱法测定盐酸多奈哌齐原料中的十种有关物质。方法应用高效液相色谱法,用十八烷基硅烷键合硅胶为填充剂的色谱柱(Inertsil ODS-3V,250 mm×4.6 mm,5μm);流动相A为磷酸溶液(取磷酸1 ml,加水1000 ml,用三乙胺调节pH值至6.60±0.05),流动相B为乙腈,流速为每分钟1.5 ml,线性梯度洗脱;柱温为50℃;检测波长为286 nm。结果在所建立的色谱条件下,系统适用性样品中十种有关物质均能完全分离,分离度≥1.9,线性回归方程为Y=11710X+6162,线性范围0.4 096～1.6 384μg/ml,精密度为0.32%,采用主成分自身对照法计算所收集的样品中各有关物质含量,杂质总量为0.1%。结论所建立的方法准确、简便、重复性好,可用于盐酸多奈哌齐原料药中十种有关物质的测定,有助于该原料及制剂的质量控制和评价。
Objective To establish a high performance liquid chromatography method for simultaneous determination of ten kinds of related substances in Donepezil Hydrochloride feedstock. Methods High performance liquid chromatography was used, and octadecylsilane chemically bonded silica was used as loading agent for chromatographic column(Inertsil ODS-3 V,250 mm×4.6 mm, 5 μm); mobile phase A was composed of phosphoric acid solution(1 ml phosphoric acid with 1000 ml water, 6.60 ±0.05 pH value adjusting by triethylamine); mobile phase B was composed of acetonitrile at 1.5 ml/min flow rate with a linear gradient elution. The column temperature was 50℃, and detection wavelength was 286 nm. Results Under the established chromatographic conditions, all 10 related substances in system suitability samples could be completely separated(resolution≥1.9). Equation of linear regression was Y=11710 X+6162 within 0.4 096-1.6 384 μg/ml of linear range and 0.32% precision. Related substances contents in collected samples were calculated by major constituent own control method. The total amount of impurities was 0.1%. Conclusion The established method is accurate, simple and well reproducible. It can be used for determination of ten kinds of related substances in Donepezil Hydrochloride, and it is helpful for quality control and evaluation of its feedstock and Donepezil Hydrochloride.
Objective To establish a high performance liquid chromatography method for simultaneous determination of ten kinds of related substances in Donepezil Hydrochloride feedstock. Methods High performance liquid chromatography was used, and octadecylsilane chemically bonded silica was used as loading agent for chromatographic column(Inertsil ODS-3 V,250 mm×4.6 mm, 5 μm); mobile phase A was composed of phosphoric acid solution(1 ml phosphoric acid with 1000 ml water, 6.60 ±0.05 pH value adjusting by triethylamine); mobile phase B was composed of acetonitrile at 1.5 ml/min flow rate with a linear gradient elution. The column temperature was 50℃, and detection wavelength was 286 nm. Results Under the established chromatographic conditions, all 10 related substances in system suitability samples could be completely separated(resolution≥1.9). Equation of linear regression was Y=11710 X+6162 within 0.4 096-1.6 384 μg/ml of linear range and 0.32% precision. Related substances contents in collected samples were calculated by major constituent own control method. The total amount of impurities was 0.1%. Conclusion The established method is accurate, simple and well reproducible. It can be used for determination of ten kinds of related substances in Donepezil Hydrochloride, and it is helpful for quality control and evaluation of its feedstock and Donepezil Hydrochloride.
引文
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[2] 傅宏义,刘倩,孙艳.多奈哌齐-阿尔茨海默病治疗新药[J].药物不良反应杂志,2002,4(1):35-37.
[3] 严秋凤,谢宁.盐酸多奈哌齐治疗老年痴呆的疗效观察[J].中南药学,2008,6(2):244-245.
[4] 陆卉,刘帅,刘淑玲,等.国产与进口盐酸多奈哌齐片治疗阿尔茨海默病的疗效比较[J].中华老年医学杂志,2015,34(1):47-50.
[5] 王梅平.美金刚联合盐酸多奈哌齐治疗阿尔茨海默病伴精神行为症状的临床效果观察[J].中国综合临床,2017,33(2):126-130.
[6] 国家药典委员会.中华人民共和国药典[M].二部.北京:中国医药科技出版社,2015:954.
[7] 刘小均,罗军波,李培海,等.RP-HPLC加校正因子的主成分自身对照法测定盐酸多奈哌齐口腔崩解片中有关物质的含量[J].中国药房,2015,26(12):1702-1705.
[8] 赵喆,唐素芳,王卫.HPLC法检查盐酸多奈哌齐制剂中的有关物质[J].中国药房,2014,25(29):2759-2761.
[9] 曹嘉,冉兰,陈霞.HPLC法检测盐酸多奈哌齐片中有关物质含量[J].中国药房,2010,21(13):1239-1240.
[10] Pappa H,Farrú R,Vilanova P O,et al.A new HPLC method to determine Donepezil hydrochloride in tablets[J].J Pharm Biomed Anal,2002,27(1-2):177-182.
[11] Kafkala S,Matthaiou S,Alexaki P,et al.New gradient high-performance liquid chromatography method for determination of donepezil hydrochloride assay and impurities content in oral pharmaceutical formulation[J].J Chromatogr A,2008,1189(1-2):392-397.