[关键词]
[摘要]
目的 分离黄精炮制过程中新产生的化学成分并研究其量变化规律。方法 采用提取分离和LC-MS法确定产生的2种化学成分的结构,通过HPLC法分析3个品种黄精炮制前后以及不同炮制时间2种成分量的变化,测定市售15个批次酒黄精中2种成分的量。HPLC色谱条件:Zorbax SB-C18色谱柱(250 mm×4.6 mm,5 μm);流动相为甲醇-水(8∶92);体积流量10 mL/min;检测波长280 nm;柱温45 ℃。结果 炮制过程中新产生的2种成分为5-羟甲基麦芽酚(DDMP)和5-羟甲基糠醛(5-HMF)。多花黄精中DDMP的量随着炮制时间的延长逐渐升高,至炮制24 h达到最高,随后开始逐渐降低;5-HMF的量随着炮制时间的延长逐渐升高。3个品种黄精炮制后均产生这2种成分。15个批次市售酒黄精中,有13个批次中DDMP的量在1.395%~5.265%,14个批次中5-HMF的量在0.079%~0.708%;自制3个品种酒黄精(16 h)中2种成分的量均在上述范围内。结论 酒黄精中2种成分的量随着炮制时间的变化而变化,研究结果为酒黄精饮片标准的制定提供依据,并为酒黄精炮制时间终点的确定提供了一定参考。
[Key word]
[Abstract]
Objective To isolate the chemical constituents newly produced in processing of Polygonati Rhizoma and to analyze the content changes during its processing. Methods Two new chemical constituents were isolated from the processed Polygonati Rhizoma by using chemical extraction and identified by LC-MS. Then HPLC analysis was performed to analyze the content changes of the two newly produced constituents in three species of wine-processed Polygonati Rhizoma during different processing periods. The contents of the two compounds in 15 batches of commercially available wine-processed Polygonati Rhizoma were determined. The HPLC was performed on a Zorbax SB-C18 column (250 mm × 4.6 mm, 5 μm) with methanol-water (8∶92) as the mobile phase at 1.0 mL/min, detection wavelength was 280 nm, and column temperature at 45 ℃. Results The newly produced chemical constituents were 2, 3-dihydro-3, 5-dihydroxy-6-methyl-4H-pyran-4-one (DDMP) and 5-hydryoxymethyl-furfural (5-HMF). The content of DDMP in Polygonatum cyrtonema increased to the top when processed to 24 h and then decreased. The content of 5-HMF was increased gradually throughout the processing. The two chemical constituents were found in the three kinds of wine-processed Polygonati Rhizoma. In the 15 batches of commercially available Polygonati Rhizoma, the range of DDMP in 13 batches was from 1.395% to 5.265%, and the range of 5-HMF in 14 batches was from 0.079% to 0.708%. Moreover, the contents of the two constituents in the three kinds of wine-processed Polygonati Rhizoma (16 h) were within the above ranges. Conclusion The contents of the two chemical constituents in Polygonati Rhizoma change with the processing time. Therefore, these results could provide the basis for making the quality standard and defining the processing time endpoint of Polygonati Rhizoma.
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[基金项目]
国家自然科学基金面上课题(81073050)