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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 |
| 阅读数： | 379 次 |
| 本月下载数： | 11 次 |
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