中国中药杂志

2020, v.45(16) 3877-3882

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HPLC-ELSD特征图谱分析地黄炮制过程成分变化
Ingredients changes in Rehmanniae Radix processing based by HPLC-ELSD specific chromatogram

张文婷;何佳;郭增喜;石上梅;
ZHANG Wen-ting;HE Jia;GUO Zeng-xi;SHI Shang-mei;Zhenjiang Institute for Food and Drug Control;NMPA Key Laboratory for Quality Evaluation of Traditional Chinese Medicine (Traditional Chinese Patent Medicine);College of Pharmaceutical Sciences, Zhejiang Chinese Medical University;Chinese Pharmacopoeia Commission;

摘要(Abstract):

建立地黄及熟地黄HPLC特征图谱分析方法,并对其化学成分进行分析比较,揭示地黄炮制过程成分变化规律。采用HPLC-ELSD,色谱柱为Prevail Carbohydrate ES(4.6 mm×250 mm,5μm),流动相为乙腈(A)-水(B)梯度洗脱,蒸发光散射检测器检测。对23批次地黄样品、25批次熟地黄样品及炮制动态样品进行比较。建立的特征图谱分析方法重复性、精密度、稳定性良好,从23批次地黄样品中提取8个共有色谱峰,25批次熟地黄样品中提取8个共有色谱峰,指认了7个色谱峰。地黄炮制过程成分比例发生较大变化,当相似度≥0.95,同时果糖峰面积为水苏糖2倍以上或果糖峰面积为棉籽糖20倍以上时的炮制程度符合经验鉴别要求。生地黄的3个主要寡糖成分,蔗糖受热生成果糖与葡萄糖,棉籽糖受热生成蜜二糖、蔗糖和果糖,水苏糖受热主要生成甘露三糖。单糖和寡糖类成分间的比例变化指标,可作为熟地黄炮制质量量化的判定标准。
To establish the HPLC-ELSD specific chromatogram analysis method of Rehmanniae Radix and Rehmanniae Radix Prae-parata, and analyze and compare their chemical compositions, so as to reveal the change regularity of compositions during the proces-sing. By HPLC-ELSD method, the chromatographic column for Prevail Carbohydrate ES(4.6 mm ×250 mm, 5 μm) was adopted, with acetonitrile(A)-water(B) as mobile phase for gradient elution, and the evaporative light-scattering detector was used. A total of 23 batches of Rehmannia Radix samples, and 25 batches of Rehmanniae Radix Praeparata samples and processing dynamic samples were compared. The established method had a great repeatability, precision and stability. Eight common chromatographic peaks were extracted from 23 batches of Rehmanniae Radix samples, 8 common peaks were extracted from 25 Rehmanniae Radix Praeparata, and 7 chromatographic peaks were identified. The composition ratio of Rehmannia Radix was changed greatly during the processing. When the simila-rity≥0.95 and the fructose peak area was more than 2 times of stachyose tetrahydrate or more than 20 times of raffinose, the processing degree conformed to the requirements of empirical identification. The three main oligosaccharides of Rehmanniae Radix were sucrose that was heated to generate fructose and glucose, stachyose tetrahydrate that was heated to generate melibiose, sucrose and fructose, and stachyose tetrahydrate that was heated to generate manninotriose. The change in the index of proportion between monosaccharides and oligosaccharides can be used as the quantitative criterion for the processing quality of Rehmanniae Radix Praeparata.

关键词(KeyWords): 地黄;熟地黄;HPLC-ELSD;特征图谱;成分比例
Rehmanniae Radix;Rehmanniae Radix Praeparata;HPLC-ELSD;fingerprint;proportion of ingredients

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作者(Author): 张文婷;何佳;郭增喜;石上梅;
ZHANG Wen-ting;HE Jia;GUO Zeng-xi;SHI Shang-mei;Zhenjiang Institute for Food and Drug Control;NMPA Key Laboratory for Quality Evaluation of Traditional Chinese Medicine (Traditional Chinese Patent Medicine);College of Pharmaceutical Sciences, Zhejiang Chinese Medical University;Chinese Pharmacopoeia Commission;

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