Fingerprint analysis of Dioscorea nipponica by high-performance liquid chromatography with evaporative light scattering detection
Fingerprint analysis of Dioscorea nipponica by high-performance liquid chromatography with evaporative light scattering detection
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DOI：
10.1016/j.aca.2006.08.057
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发表时间：
2007-01-16
影响因子：
6.2
通讯作者：
Yan, Qiong
中科院分区：
文献类型：
--
作者：
Liu, Chun-Zhao;Zhou, Hua-Ying;Yan, Qiong
高效液相色谱法 (HPLC) 结合蒸发光散射检测 (ELSD) 与微波辅助萃取 (MAE) 作为一种有效的样品制备技术，已开发用于薯蓣指纹图谱分析。采用 Agilent C8 色谱柱，以水 (A) 和乙腈 (13) 在梯度条件（0-10 min，线性梯度 20-40% B；10-12 min，线性梯度 40-42% B；12-25 min，等度 42% B）为流动相，流速 1 mL min(-1)，在 22 min 内分离样品。 ELSD条件优化为雾化器气体流量2.7 L min(-1)、漂移管温度90℃。精密实验表明峰面积和保留时间的相对标准偏差(R.S.D.)优于2.5%；日间和日内变异表明 R.S.D.范围为 0.78% 至 4.74%。检出限小于50μg·mL(-1)，定量限小于80μg·mL(-1)。准确度验证表明平均回收率在 97.39% 至 104.07% 之间。经验证该方法达到了令人满意的精密度和回收率。相对保留时间和相对峰面积用于识别指纹分析的共同峰。指纹中有九个共同峰。以共有峰的“差值”和“总差值”参数评定7批日本石竹样品的质量合格与不合格。此外，利用所开发的HPLC-ELSD方法同时测定了不同批次的日本石竹样品中重要药用化合物（薯蓣皂苷、原薯蓣皂苷和纤细素）的含量。结果表明，药材品质存在差异，可能与不同产地、生长条件、气候、采收时间、药物加工等有关。所开发的分析程序被证明是一种可靠且快速的日本石斛质量控制方法。 (c) 2006 Elsevier B.V. 保留所有权利。
High-performance liquid chromatographic method (HPLC) with evaporative light scattering detection (ELSD) coupled with microwave-assisted extraction (MAE) as an efficient sample preparation technique has been developed for fingerprint analysis of Dioscorea nipponica. The samples were separated with an Agilent C8 column using water (A) and acetonitrile (13) under gradient conditions (0-10 min, linear gradient 20-40% B; 10-12 min, linear gradient 40-42% B; 12-25 min, isocratic 42% B) as the mobile phase at a flow rate of 1 mL min(-1) within 22 min. The ELSD conditions were optimized at nebulizer-gas flow rate 2.7 L min(-1) and drift tube temperature 90 degrees C. Precision experiments showed relative standard deviation (R.S.D.) of peak area and retention time were better than 2.5%; inter-day and intra-day variabilities showed that R.S.D. was ranged from 0.78% to 4.74%. Limit of detection was less than 50 mu g mL(-1) and limit of quantification was less than 80 mu g mL(-1). Accuracy validation showed that average recovery was between 97.39% and 104.07%. The method was validated to achieve the satisfactory precision and recovery. Relative retention time and relative peak area were used to identify the common peaks for fingerprint analysis. There are nine common peaks in the fingerprint. The quality of seven batches of D. nipponica samples was evaluated to be qualified or unqualified by the parameters "difference" and "total difference" of common peaks. Furthermore, the contents of important medicinal compounds (dioscin, prodioscin and gracillin) in different batches of D. nipponica samples were determined simultaneously using the developed HPLC-ELSD method. The results indicated variation of the herb quality which might be related to different producing area, growing condition, climate, harvest time, drug processing and so on. The developed analytical procedure was proved to be a reliable and rapid method for the quality control of D. nipponica. (c) 2006 Elsevier B.V. All rights reserved.