Chemical fingerprinting of Liuwei Dihuang Pill and simultaneous determination of its major bioactive constituents by HPLC coupled with multiple detections of DAD, ELSD and ESI-MS
Chemical fingerprinting of Liuwei Dihuang Pill and simultaneous determination of its major bioactive constituents by HPLC coupled with multiple detections of DAD, ELSD and ESI-MS
复制标题
DOI：
10.1016/j.jpba.2008.12.009
复制
发表时间：
2009-04-05
影响因子：
3.4
通讯作者：
Zhang, Weidong
中科院分区：
文献类型：
--
作者：
Ye, Ji;Zhang, Xi;Zhang, Weidong
为控制六味地黄丸的质量，建立了高效液相色谱-多检测器联用技术（HPLC-Multiple Detection Techniques）指纹图谱分析方法，并同时测定了六味地黄丸中多种活性成分的含量。采用高效液相色谱-紫外检测法（HPLC-UV）建立其指纹图谱，采用高效液相色谱-二极管阵列检测器-蒸发光散射检测器（HPLC-DAD-ELSD）同时测定没食子酸、5-羟甲基糠醛、莫诺苷、当药苷等8种活性成分。马钱苷、芍药苷、丹皮酚和泽泻醇B-23乙酸酯。方法的检出限和定量限为0.11-1.93 μ g/ml。和0.38-3.85 μ g/mL。回收率试验结果表明，该方法的准确率为93.47-104.62%，验证结果令人满意。方法的日内和日间精密度均小于3.87%，准确度为95.3%~ 103.4%。此外，还对所研究的主要成分进行了质谱分析。基于色谱指纹图谱数据，采用偏最小二乘法（PLS）和判别分析对60批LDP的质量信息进行可视化，建立了具有较好预测性能的偏最小二乘法-判别分析（PLS-DA）模型。建议的方法有望被开发为LDR（C）2008 Elsevier B. V.质量控制的有力工具。
For quality control purpose, an approach of chemical fingerprinting of Liuwei Dihuang Pill (LDP) and simultaneous determination of its multiple bioactive components were established by using high performance liquid chromatograph (HPLC)coupled with multiple detection techniques. HPLC with ultraviolet detection (HPLC-UV) was used to acquire its fingerprint, and HPLC with combined detections of diode array detector and evaporative light scattering detector (HPLC-DAD-ELSD) was performed to simultaneously determine eight bioactive constituents: including gallic acid, 5-hydroxymethyl furfural, morroniside, sweroside. loganin, paeoniflorin, paeonol and alisol B-23 acetate. The detection limits and quantification limits ranged in 0.11-1.93 mu g/ml. and 0.38-3.85 mu g/mL, respectively. The validation of the proposed approach was acceptable, with 93.47-104.62% accuracy in recovery test. The intra- and inter-day precisions of the method were evaluated and were less than 3.87%, with accuracy from 95.3% to 103.4%. In addition, the mass spectrometry of the investigated major constituents was also studied. Based on the chromatographic fingerprint data, partial least square (PLS) and discriminate analysis were utilized to visualize the quality information of 60 batches of LDP, and a partial least square-discriminate analysis (PLS-DA) model was constructed with acceptable predictive performance for the discrimination of various products. The proposed approach was expected to be developed as a powerful tool for the quality control of LDR (C) 2008 Elsevier B.V. All rights reserved.