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用于同时分析(Roxb. ex Willd.)地上部分中岩白菜素和山荷叶素的超高效液相色谱-光电二极管阵列检测法的建立与验证

Development and validation of UPLC-PDA method for concurrent analysis of bergenin and menisdaurin in aerial parts of (Roxb. ex Willd.).

作者信息

Hussain Afzal, Alam Perwez, Siddiqui Nasir Ali, Alajmi Mohamed Fahad, Rehman Md Tabish, Kalam Mohd Abul, Al-Rehaily Adnan Jathlan

机构信息

Department of Pharmacognosy, College of Pharmacy, King Saud University, P.O. Box-2457, Riyadh 11451, Saudi Arabia.

Nanomedicine Research Unit, Department of Pharmaceutics, College of Pharmacy, King Saud University, Riyadh 11451, Saudi Arabia.

出版信息

Saudi Pharm J. 2018 Nov;26(7):970-976. doi: 10.1016/j.jsps.2018.05.007. Epub 2018 May 22.

Abstract

Bergenin and menisdaurin are biologically active components which are found in plant (Phyllanthaceae). Bergenin has pharmacological actions such as chemopreventive and antihepatotoxic while menisdaurin has an anti-viral activity which needs its evaluation by an analytical method (UPLC-PDA method) that can be applied to the quality control of pharmaceutical preparations. The developed UPLC-PDA method was applied for identification and quantification of standards bergenin and menisdaurin in the methanol extract of (FVME). The analysis was carried out using Eclipse C18 (4.6 × 100 mm, 3.5 µm) UPLC column. The optimized chromatographic condition was achieved at 0.16 mL/min flow rate using gradient system with acetonitrile and water as mobile phase. Both biomarkers were measured at λ 235 nm in PDA detector at ambient temperature. The developed method furnished sharp and intense peaks of menisdaurin and bergenin at Rt = 2.723 and 3.068 min, respectively along with r2 > 0.99 for both. The recoveries of bergenin and menisdaurin were found in the range of 99.37-101.49% and 98.20-100.08%, respectively. With other validation data, including precision, specificity, accuracy, and robustness, this method demonstrated excellent reliability and sensitivity. The separation parameters i.e. retention, separation, and resolution factors for resolved standards (bergenin and menisdaurin) were >1, which showed good separation. The quantity of bergenin and menisdaurin in the FVME sample was found as 15.16 and 3.28% w/w, respectively. The developed UPLC-PDA method could be conveniently adopted for the routine quality control analysis.

摘要

岩白菜素和蛇莓苷是在叶下珠科植物中发现的生物活性成分。岩白菜素具有化学预防和抗肝毒性等药理作用,而蛇莓苷具有抗病毒活性,需要通过一种可应用于药物制剂质量控制的分析方法(超高效液相色谱 - 光电二极管阵列检测法,UPLC - PDA法)对其进行评估。所开发的UPLC - PDA法用于鉴定和定量叶下珠甲醇提取物(FVME)中的岩白菜素和蛇莓苷标准品。分析使用Eclipse C18(4.6×100 mm,3.5 µm)超高效液相色谱柱进行。在以乙腈和水为流动相的梯度系统中,以0.16 mL/min的流速实现了优化的色谱条件。两种生物标志物在室温下的PDA检测器中于λ 235 nm处进行测定。所开发的方法分别在Rt = 2.723和3.068分钟时给出了尖锐且峰形良好的蛇莓苷和岩白菜素峰,两者的r2均> 0.99。岩白菜素和蛇莓苷的回收率分别在99.37 - 101.49%和98.20 - 100.08%的范围内。结合包括精密度、特异性、准确性和稳健性在内的其他验证数据,该方法显示出出色的可靠性和灵敏度。分离标准品(岩白菜素和蛇莓苷)的分离参数,即保留因子、分离因子和分辨率因子均>1,表明分离效果良好。FVME样品中岩白菜素和蛇莓苷的含量分别为15.16% w/w和3.28% w/w。所开发的UPLC - PDA法可方便地用于常规质量控制分析。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9538/6218377/79dc768b20aa/gr1.jpg

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