非达霉素原料药中有关物质的检查方法研究
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篇名: 非达霉素原料药中有关物质的检查方法研究
TITLE: Study on Detection Methods for Related Substances in Fidaxomicin Raw Material
摘要: 目的:建立非达霉素原料药中有关物质的检查方法。方法:分别考察正相-紫外检测器色谱系统、反相-蒸发光散射检测器色谱系统、反相-紫外检测器色谱系统对非达霉素原料药中有关物质的检出能力,优选出最佳色谱系统。建立有关物质检查的高效液相色谱法,色谱柱为AgilentEclipseXDBC18,流动相A为0.2%三乙胺缓冲液(pH3.8)-乙腈(55∶45,V/V)、流动相B为0.2%三乙胺缓冲液(pH3.8)-乙腈(20∶80,V/V)(梯度洗脱),流速为1.0mL/min,检测波长为230nm,柱温为35℃,进样量为10µL;以不加校正因子的主成分自身对照法计算有关物质含量。结果:非达霉素在正相-紫外检测器色谱系统下不能有效分离杂质C、F,在反相-蒸发光散射检测器色谱系统下仅能检出杂质C、D、E、F4个杂质;在反相-紫外检测器色谱系统下可检出11个杂质,故以此系统进行有关物质检查。在方法学考察中,非达霉素检测质量浓度线性范围为0.5~20.0μg/mL(R2=0.9999);检测限为0.05ng,定量限为0.15ng;重复性、中间精密度试验的RSD均小于2.0%(n=6);平均回收率为98.4%(RSD为3.6%,n=9)。3批非达霉素原料药中杂质含量分别为0.53%、0.51%、0.51%。结论:非达霉素在反相-紫外检测器色谱系统下进行杂质检查效果最好;建立的有关物质检查方法专属性强、灵敏度高,可用于非达霉素原料药中有关物质的检查。
ABSTRACT: OBJECTIVE:To establish th e method for the determination of related substances in fidaxomicin raw material. METHODS:The detection ability of NP-HPLC-UV ,RP-HPLC-ELSD and RP-HPLC-UV systems for the related substances in fidamycin raw material was investigated and the best chromatographic system was selected . The HPLC detection method for the related substances was established. The detection was performed on Agilent Eclipse XDB C 18 column with mobile phase A consisted of 0.2% triethylamine buffer solution (pH 3.8)-acetonitrile(55∶45,V/V),mobile phase B consisted of 0.2% triethylamine buffer solution(pH 3.8)-acetonitrile(20∶80,V/V)at the flow rate of 1.0 mL/min(gradient elution );the detection wavelength was set at 230 nm,and column temperature was 35 ℃;the sample size was 10 µL. Calculation of the content of related substances was principal component self-control method without correction factor. RESULTS :The impurities C and F could not be separated effectively in NP-HPLC-UV system. In RP-HPLC-ELSD system ,only impurities C ,D,E and F could be detected. In RP-HPLC-UV system ,11 impurities could be detected. In the study of methodology ,the linear ranges were 0.5-20.0 μg/mL for fidaxomicin(R2=0.999 9);the LOD was 0.05 ng,LOQ was 0.15 ng;RSDs of reproducibility and intermediate precision tests were less than 2.0%(n=6);average recovery was 98.4%(RSD=3.6%,n=9). The sum of impurities in 3 batches of raw materials were 0.53%,0.51%,0.51%,respectively. CONCLUSIONS :The effect of detecting impurities by RP-HPLC-UV are the best. Established method is specific and sensitive ,and can be used for the determination of related substance in fidaxomicin raw material.
期刊: 2020年第31卷第05期
作者: 王娅莉,刘月,班璐,李晓露,程晓昆,任风芝,张雪霞
AUTHORS: WANG Yali,LIU Yue,BAN Lu,LI Xiaolu ,CHENG Xiaokun ,REN Fengzhi ,ZHANG Xuexia
关键字: 非达霉素;高效液相色谱法;正相色谱;反相色谱;紫外检测器;蒸发光散射检测器;主成分自身对照法;有关物质
KEYWORDS: Fidaxomicin;HPLC;Normal phase chromatogram ;Reverse phase chromatogram ;UV detector ;ELSD;Principal
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