[關(guān)鍵詞]
[摘要]
目的 建立靈芝提取物中中性三萜——靈芝醇A、靈芝醛A、靈芝酮三醇及麥角甾醇的超高效液相色譜(UPLC)定量分析方法及一測多評法。方法 甲醇超聲提取法制備靈芝提取物;超高效液相色譜(UPLC)法采用PhenomenexLuna Omega PS C18色譜柱(150 mm×2.1 mm,1.6 μm),流動相為乙腈-0.04%甲酸溶液,梯度洗脫,檢測波長254 nm,柱溫30℃;一測多評法應(yīng)用靈芝醇A作為內(nèi)參物,計算靈芝醛A、靈芝酮三醇及麥角甾醇的相對校正因子;精密吸取10批靈芝供試品溶液進樣檢測,比較建立的外標(biāo)法與一測多評法結(jié)果是否一致。結(jié)果 4種成分在設(shè)定的質(zhì)量范圍內(nèi)線性關(guān)系良好(r≥0.998 8),方法的精密度、重復(fù)性、穩(wěn)定性的RSD均小于2.13%,加樣回收率在92%~105%、RSD均小于1.99%,準(zhǔn)確度良好;靈芝醛A、靈芝酮三醇及麥角甾醇的相對校正因子分別為1.02、0.99、1.80,一測多評法和外標(biāo)法測定結(jié)果差異不大。結(jié)論 建立的測定靈芝中靈芝醇A、靈芝醛A、靈芝酮三醇和麥角甾醇UPLC外標(biāo)法和一測多評法的專屬性強,便捷高效,結(jié)果準(zhǔn)確,適用于靈芝提取物中性三萜的定量分析。
[Key word]
[Abstract]
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, 1.6 μm), 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 ≥ 0.998 8), 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.
[中圖分類號]
R284.1
[基金項目]
福建省科技計劃區(qū)域發(fā)展項目(2020N3002);福建省技術(shù)創(chuàng)新重點攻關(guān)及產(chǎn)業(yè)化項目(2022G028)