Simultaneous determination of nine major active compounds in Dracocephalum rupestre by HPLC
Simultaneous determination of nine major active compounds in Dracocephalum rupestre by HPLC
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HPLC法同时测定青兰中9种主要活性成分
DOI：
10.1016/j.jpba.2008.09.013
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发表时间：
2008-12-15
影响因子：
3.4
通讯作者：
Lou, Hong-Xiang
中科院分区：
文献类型：
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作者：
Rena, Dong-Mei;Qu, Zhi;Lou, Hong-Xiang
建立了青兰中9种主要成分的同时测定方法，包括5,7-二羟基色酮(1)、圣草酚-7-O-β-D-葡萄糖苷(2)、木犀草素-7-O-β-D-葡萄糖苷(3)、柚皮素-7-O-β-D-葡萄糖苷(4)、芹菜素-7-O-β-D-葡萄糖苷 (5)、圣草酚 (6)、木犀草素 (7)、柚皮素 (8) 和芹菜素 (9)。采用光电二极管阵列检测器反相高效液相色谱法（LC-PDA）进行定量测定。在 Agilent Eclipse XDB-C-18 柱（150 mm x 4.6 mm 内径，5 μm）上进行分离，采用乙腈和 0.5% 乙酸水溶液梯度洗脱。通过保留时间、紫外 (UV) 光谱鉴定成分，并通过 LC-PDA 在 260 nm 处进行定量。所有校准曲线在测试范围内均表现出良好的线性 (r(2) > 0.999)。通过日内和日间测定以及 R.S.D 评估重现性。值均小于 3.0%。回收率在 95.15% 至 104.45% 之间。检测限 (LOD) 范围为 0.002 至 0.422 μg/ml，定量限 (LOQ) 范围分别为 0.005 至 1.208 μg/ml。通过配备三重四极杆质谱系统和电喷雾电离（ESI）接口的高效液相色谱进一步证实了峰的身份。所开发的方法用于测定不同采收时间收集的 14 个石榴样品中的 9 种成分。大多数化合物在六月至七月左右的积累量要高得多。令人满意的结果表明所开发的方法很容易用作石榴的质量控制方法。 (C) 2008 Elsevier B.V. 保留所有权利。
A new method was developed for the simultaneous determination of nine major constituents in Dracocephalum rupestre, including 5,7-dihydroxychromone (1), eriodictyol-7-O-beta-D-glucoside (2), luteolin-7-O-beta-D-glucoside (3), naringenin-7-O-beta-D-glucoside (4), apigenin-7-O-beta-D-glucoside (5), eriodictyol (6), luteolin (7), naringenin (8) and apigenin (9). The quantitative determination was conducted by reversed phase high-performance liquid chromatography with photodiode array detector (LC-PDA). Separation was performed on an Agilent Eclipse XDB-C-18 column (150 mm x 4.6 mm i.d., 5 mu m) with gradient elution of acetonitrile and 0.5% aqueous acetic acid. The components were identified by retention time, ultraviolet (UV) spectra and quantified by LC-PDA at 260 nm. All calibration curves showed good linearity (r(2) > 0.999) within test ranges. The reproducibility was evaluated by intra- and inter-day assays and R.S.D. values were less than 3.0%. The recoveries were between 95.15 and 104.45%. The limits of detection (LOD) ranged from 0.002 to 0.422 mu g/ml and limits of quantification (LOQ) ranged from 0.005 to 1.208 mu g/ml, respectively. The identity of the peaks was further confirmed by high- performance liquid chromatography with triple-quadrupole mass spectrometry system coupled with electrospray ionization (ESI) interface. The developed method was applied to the determination of nine constituents in 14 samples of D. rupestre collected at various harvesting times. Most compounds accumulated at much higher amounts in about June-July. The satisfactory results indicated that the developed method was readily utilized as a quality control method for D. rupestre. (C) 2008 Elsevier B.V. All rights reserved.