4-去甲基-柔红霉素标准物质的研制

Development of national reference standard of 4-demethyl-daunorubicin hydrochloride

目的:为满足国内盐酸伊达比星质量控制需要,对《中华人民共和国药典》2020年版标准中盐酸伊达比星系统适用性杂质4-去甲基-柔红霉素进行标定研制。方法:采用MS和NMR等技术对4-去甲基-柔红霉素标准物质的结构进行确证,并首次对该化合物的核磁信号进行了准确归属。采用质量平衡法确定了4-去甲基-柔红霉素的含量,并进一步利用核磁定量法对上述结果进行佐证。结果:本批4-去甲基-柔红霉素标准物质的含量按盐酸4-去甲基-柔红霉素(C_(26)H_(27)NO_(10)·HCl)计为91.5%。结论:建立了首批4-去甲基-柔红霉素标准物质。

Objective: In order to satisfy the quality control of idarubicin hydrochloride products in Chinese market, the calibration development of 4-demethyl-daunorubicin for system suitability in the “Chinese Pharmacopoeia” 2020 edition was carried out. Methods: The structure of 4-demethyl-daunorubicin hydrochloride was identified by LC-MS and NMR. The nuclear magnetic signals of the compound were accurately assigned for the first time. The content of 4-demethyl-daunorubicin hydrochloride was determined using mass balance method, which was further approved by quantitative nuclear magnetic resonance(QNMR). Results:The content of 4-demethyl-daunorubicin was calculated by 4-demethyl-daunorubicin hydrochloride(C_(26)H_(27)NO_(10)·HCl) reference standard, which is 91.5%. Conclusion: The first batch of national standard substances of 4-demethyl-daunorubicin hydrochloride was successfully developed.