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HPLC法测定贝林司他中有关物质的含量
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篇名: HPLC法测定贝林司他中有关物质的含量
TITLE: Content Determination of Related Substances in Belinostat by HPLC
摘要: 目的:建立贝林司他中有关物质的含量测定方法。方法:采用高效液相色谱法检测并以加校正因子的主成分自身对照法进行计算。以ODS-AM为色谱柱,以1.02%磷酸二氢钾缓冲液(用磷酸调节pH值至3.5)-乙腈(85∶15,V/V)为流动相A、1.02%磷酸二氢钾缓冲液(用磷酸调节pH值至3.5)-乙腈(30∶70,V/V)为流动相B进行梯度洗脱,流速为1.0mL/min,柱温为30℃,检测波长为220nm,进样量为10μL。结果:贝林司他及杂质A、D、F、G、H的线性范围分别为0.113~1.693、0.050~1.496、0.117~1.750、0.098~1.471、0.120~1.799、0.100~1.506μg/mL(r≥0.9997),后5个杂质的校正因子分别为1.0、1.0、1.2、1.5、1.0;检测限分别为0.250、0.590、0.490、0.600、0.500ng,定量限分别为0.500、1.170、0.980、1.200、1.000ng,回收率为90.18%~111.48%(RSD为1.52%~4.78%,n=9),稳定性(100h)、精密度试验的RSD均不大于16%,耐用性良好。3批贝林司他原料药中检测出杂质A、D、H,含量分别为0.030%~0.038%、0.019%~0.022%、0.012%~0.013%,其他最大单体杂质含量为0.012%~0.013%,总杂质含量为0.075%~0.084%,未检出杂质B、C、F、G。结论:成功建立了测定贝林司他中有关物质含量的方法,且方法准确、专属性好。
ABSTRACT: OBJECTIVE:To establish the method for the con tent determination of related substances in belinstat. METHODS : HPLC method was adopted and the principal component self-control comparison method with correction factor was used to calculate the contents of related substances. The determination was performed on ODS-AM column with 1.02% potassium dihydrogen phosphate buffer (pH value adjusted to 3.5 with phosphoric acid )-acetonitrile(85∶15,V/V)as mobile phase A ,1.02% potassium dihydrogen phosphate buffer (pH value adjusted to 3.5 with phosphoric acid )-acetonitrile(30 ∶ 70,V/V)as mobile phase B (gradient elution ),at the flow rate of 1.0 mL/min. The column temperature was set at 30 ℃,and the detection wavelength was 220 nm. The sample size was 10 μL. RESULTS:The linear ranges of belinstat and impurities A ,D,F,G,H were 0.113-1.693, 0.050-1.496,0.117-1.750,0.098-1.471,0.120-1.799,0.100-1.506 μ g/mL(r≥0.999 7). The correction factors of the last 5 impurities were 1.0,1.0,1.2,1.5,1.0;the detection limits were 0.250,0.590,0.490,0.600,0.500 ng,respectively. The quantification limits were 0.500,1.170,0.980,1.200,1.000 ng,respectively. The recoveries were 90.18%-111.48%(RSD= 1.52%-4.78%,n=9). RSDs of stability (100 h)and precision tests were no more than 16%,and the durability was good. Impurities A ,D and H were detected in 3 batches of belinlestat ,the contents were 0.030%-0.038%,0.019%-0.022% and 0.012%-0.013%,respectively. The contents of other maximum monomer impurities were 0.012%-0.013% and the total impurities were 0.075%-0.084%. Impurities B ,C,F,G were not detected. CONCLUSIONS :The method for the content determination of related substances in belinstat has been successfully established ,and the method is accurate and specific.
期刊: 2021年第32卷第08期
编辑: 孙朋杰,张莉,杜超,李伟,卓秋琪
AUTHORS: SUN Pengjie ,ZHANG Li,DU Chao,LI Wei,ZHUO Qiuqi
关键字: 贝林司他;有关物质;高效液相色谱法;加校正因子的主成分自对照法
KEYWORDS: Belinostat;Related substances ;HPLC;Principal component self-control comparison method wit h correct ion factor
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