摘要
目的建立灵芝提取物中中性三萜——灵芝醇A、灵芝醛A、灵芝酮三醇及麦角甾醇的超高效液相色谱(UPLC)定量分析方法及一测多评法。方法甲醇超声提取法制备灵芝提取物;超高效液相色谱(UPLC)法采用Phenomenex Luna Omega PS C18色谱柱(150 mm×2.1 mm,1.6μm),流动相为乙腈-0.04%甲酸溶液,梯度洗脱,检测波长254 nm,柱温30℃;一测多评法应用灵芝醇A作为内参物,计算灵芝醛A、灵芝酮三醇及麦角甾醇的相对校正因子;精密吸取10批灵芝供试品溶液进样检测,比较建立的外标法与一测多评法结果是否一致。结果4种成分在设定的质量范围内线性关系良好(r≥0.9988),方法的精密度、重复性、稳定性的RSD均小于2.13%,加样回收率在92%~105%、RSD均小于1.99%,准确度良好;灵芝醛A、灵芝酮三醇及麦角甾醇的相对校正因子分别为1.02、0.99、1.80,一测多评法和外标法测定结果差异不大。结论建立的测定灵芝中灵芝醇A、灵芝醛A、灵芝酮三醇和麦角甾醇UPLC外标法和一测多评法的专属性强,便捷高效,结果准确,适用于灵芝提取物中性三萜的定量分析。
Objective To establish an quantitative analysis method and QAMS by UPLC for ganoderol A,ganoderal A,ganodermanontriol and ergosterol from Ganoderma Lucidum extract.Methods The UPLC content determination was performed on a Phenomenex Luna Omega PS C18 chromatographic column(150 mm×2.1 mm,1.6μm),with acetonitrile-0.04%formic acid as the mobile phase,the detection wave was set at 254 nm,the column temperature was 30℃.QAMS used ganoderal A as the internal reference material to calculate the relative correction factors of ganoderal A,ganodermanontriol and ergosterol.Precisely aspirate 10 batches of Ganoderma lucidum test solution for injection testing,and compare the results of the established external standard method and QAMS for consistency.Result The results showed that the 4 components established a good linear relationship(r≥0.9988),and the relative standard deviations(RSD)of precision,stability,and repeatability were all less than 2.13%,and the recovery rate was 92%—105%,RSD was less than 1.99%,the accuracy of this method was good.The relative correction factors for ganoderal A,ganodermanontriol and ergosterol were 1.02,0.99,and 1.80,respectively.There was no significant difference in the results between the one test multiple evaluation method and the external standard method.Conclusion The UPLC determination method and QAMS of neutral triterpenoids and ergosterol in this study is specific,simple,efficient and accurate,which is suitable for the quantitative analysis of Ganoderma neutral triterpenoids and ergosterol.
作者
金凌云
陈言枧
洪丽玲
郑德辉
周岩飞
吴长辉
李晔
JIN Lingyun;CHEN Yanjian;HONG Liling;ZHENG Dehui;ZHOU Yanfei;WU Changhui;LI Ye(Fujian Xianzhilou Biological Science&Technology Co.Ltd,Research Center of Medicinal Mushroom Cultivation and Deep Processing of Local National United Engineering,National R&D Branch Center for Edible Fungi Processing,Fuzhou 350108,China;Fujian University of Traditional Chinese Medicine,Fuzhou 350122,China)
出处
《药物评价研究》
CAS
2023年第11期2380-2386,共7页
Drug Evaluation Research
基金
福建省科技计划区域发展项目(2020N3002)
福建省技术创新重点攻关及产业化项目(2022G028)。
关键词
灵芝提取物
中性三萜
定量分析
一测多评
超高效液相色谱法
灵芝酮三醇
灵芝醇A
灵芝醛A
麦角甾醇
Ganoderma lucidum extract
neutral triterpenoids
quantitative analysis
QAMS
ultra-performance liquid chromatography(UPLC)
ganodermanontriol
ganoderol A
ganoderal A
ergosterol
