[1]杨兰,李欠,冯彦梅,等.定量核磁共振波谱法测定白芷中欧前胡素含量[J].江苏农业学报,2020,(04):1049-1053.[doi:doi:10.3969/j.issn.1000-4440.2020.04.034]
　YANG Lan,LI Qian,FENG Yan-mei,et al.Determination of imperatorin in Angelica dahuricae by quantitative nuclear magnetic resonance (qNMR) spectroscopy[J].,2020,(04):1049-1053.[doi:doi:10.3969/j.issn.1000-4440.2020.04.034]
点击复制

定量核磁共振波谱法测定白芷中欧前胡素含量()
分享到：

江苏农业学报[ISSN:1006-6977/CN:61-1281/TN]

卷:
期数:
2020年04期
页码:
1049-1053
栏目:
加工贮藏·质量安全
出版日期:
2020-08-31

文章信息/Info

Title:
Determination of imperatorin in Angelica dahuricae by quantitative nuclear magnetic resonance (qNMR) spectroscopy
作者:
杨兰; 李欠; 冯彦梅; 邱黛玉
(甘肃农业大学农学院中草药栽培与鉴定系，甘肃省中药材规范化生产技术创新重点实验室，甘肃兰州730070）
Author(s):
YANG Lan; LI Qian; FENG Yan-mei; QIU Dai-yu
(Department of Cultivation and Identification of Chinese Herbal Medicine, Gansu Provincial Key Laboratory of Good Agricultural Productive Technology for Traditional Chinese Medicines, College of Agronomy, Gansu Agricultural University, Lanzhou 730070, China)
关键词:
白芷; 欧前胡素; 定量核磁共振波谱法; 高效液相色谱法
Keywords:
Angelica dahuricae; imperatorin; quantitative nuclear magnetic resonance (qNMR) spectroscopy; high performance liquid chromatography (HPLC)
分类号:
R284.1
DOI:
doi:10.3969/j.issn.1000-4440.2020.04.034
文献标志码:
A
摘要:
为建立定量核磁共振波谱法测定白芷中欧前胡素含量的方法，以对苯二酚为内标、氘代二甲基亚砜(DMSO-d6)为溶剂，在400 MHz光谱仪上进行了qNMR测量。选择测定温度为293.7 K，谱宽(SWH)为8 012.8 Hz，采样时间(AQ)为4.0 s，弛豫时间(D1)为1 s，脉冲宽度(P1) 14.90 s，扫描次数(NS)为32次，空扫次数(DS)为2次，以欧前胡素中δ7.65的峰为定量峰，对苯二酚中δ6.55的峰为内标定量峰。对线性关系、检测限、定量限、精密度、重复性、稳定性和回收率等进行了方法学评价，结果良好。采用高效液相色谱法加以验证，2种方法测定结果基本一致，表明qNMR可用于白芷中欧前胡素含量测定。
Abstract:
A quantitative nuclear magnetic resonance (qNMR) spectroscopy for determining the imperatorin content in traditional Chinese medicine Angelica dahuricae was established. The qNMR measurements were performed on 400 MHz spectrometer with hydroquinone as the internal standard reference in deuterated dimethyl sulfoxide (DMSO-d6) solvent. The temperature was 293.7 K, spectral width (SWH) was 8 012.8 Hz, sampling time (AQ) was 4.0 s, relaxation time (D1) was 1 s, pulse width (P) was 14.90 s, the number of scans (NS) was 32 times, the number of empty sweep (DS) was two times. The peak of δ7.65 in imperatorin and the peck of δ6.55 in hydroquinone were selected as quantitative peak and internal standard peak, respectively． The linearity, detection limit, the limit of quantification, precision, reproducibility, stability and recovery were evaluated by methodology, and results were good. The obtained results were validated by high performance liquid chromatography (HPLC) method. The determined contents of imperatorin by qNMR are in accordance with the results by HPLC，indicating that qNMR can be applied to determine imperatorin of Angelica dahuricae.

参考文献/References:

[1]赵亮,曹红.白芷有效成分提取工艺的优化及其中药材质量研究[J].现代生物医学进展,2011,11(14):2759- 2766，2774.
[2]崔秋兵,张艺,兰莎.白芷镇痛作用物质基础研究[J].中国实验方剂学杂志,2010,16(12):102-104.
[3]周淑敏.白芷香豆素的提取及其抑菌活性研究[J].食品工业,2014,35(3):141-144.
[4]王方,王灿.白芷醇提物延缓皮肤衰老与抗氧化作用的相关性研究[J].中国药房,2012,23(7):599-602.
[5]韦玮,徐嵬,杨秀伟,等.杭白芷醋酸乙酯部位化学成分研究[J].中草药,2016,47(15):2606-2613.
[6]LIANG W H, CHANG T W, CHARNG Y C. Effects of drying methods on contents of bioactive compounds and antioxidant activities of Angelica dahuricae[J]. Food Sci Biotechnol, 2018, 27(4): 1085-1092.
[7]JIANG Y, LU X, PENG W, et al. Study on the influence of sulfur fumigation on chemical constituents of Angelica dahuricae Radix (Baizhi) [J]. Trop J Pharm Res, 2015, 14 (5): 815.
[8]KANG J, ZHOU L, SUN J, et al. Chromatographic fingerprint analysis and characterization of furocoumarins in the roots of Angelica dahuricae by HPLC/DAD/ESI-MSn technique[J]. J Pharmaceu Biomed, 2008, 47(4/5):778-785.
[9]邓改改,崔治家,杨秀伟.川白芷根极性化学成分研究[J].中国中药杂志,2015, 40(19):3805-3810.
[10]郑立辉,王鹏君,李伟,等.白芷精油成分分析及清除DPPH自由基活性[J].食品科学,2014,35 (14):180-183.
[11]WANG J, LIAN P, YU Q, et al. Purification, characterization and procoagulant activity of polysaccharides from Angelica dahuricae roots[J]. Chem Cent J, 2017，11(1):17.
[12]FAN G, DENG R, ZHOU L, et al. Development of a rapid resolution liquid chromatographic method combined with chemometrics for quality control of Angelica dahuricae radix[J]. Phytochem Analysis, 2011, 23(4):299-307.
[13]中华人民共和国国家药典委员会.中华人民共和国药典[M].北京:中国医药科技出版社,2015:105-106.
[14]王志伟,闫慧娇,王晓,等.氢核磁共振法测定中药茜草中大叶茜草素和羟基茜草素的含量[J].山东科学, 2017,30(1):1-7.
[15]林珊,苏娟,叶霁,等.定量核磁共振技术在中药分析中的应用进展[J].药学实践杂志,2014,32(2):92-95，106.
[16]禹珊.定量核磁共振波谱法分析中药虎杖和板蓝根中的有效成分[D].上海:上海应用技术学院,2015.
[17]王思寰,郝海军,王广东,等.氢核磁共振定量法测定黄藤素含量[J].药物分析杂志,2017,37(4):654-658.
[18]黄海伟,何兰,岳昊坤,等.氢核磁共振定量法测定恩替卡韦[J].药物评价研究,2015,38(5):520-522.
[19]OWCZAREK A, KLYS A, OLSZEWSKA M A. A validated 1H-qNMR method for direct and simultaneous quantification of esculin, fraxin and (-)-epicatechin in Hippocastani cortex[J]. Talanta, 2019, 192: 263-269.
[20]禹珊,郭强胜,王会琳,等.定量核磁共振波谱法同时测定中药虎杖中白藜芦醇和虎杖苷的含量[J].分析化学, 2015,3(1):69-74.
[21]王志伟,闫慧娇,陈跃,等.氢核磁共振法测定何首乌中大黄素和大黄素甲醚的含量[J].药物分析杂志,2016, 36(12):2163-2167.
[22]陈燕燕,李晓男,王跃飞,等.解卷积定量核磁共振法测定黄芪注射液中8种初生代谢成分[J].分析化学, 2015,43(8):1210-1217.
[23]陈夏霖,耿婷,黄文哲,等.基于1H-NMR技术的银杏二萜内酯原料药含量测定和指纹图谱研究[J].中国中药杂志,2018,43(7):1404-1409.
[24]张继远,樊小瑞,刘晓谦,等.核磁共振氢谱内标法测定常山碱的绝对含量[J].中国中药杂志,2018,43(1): 134-138.
[25]杨应文,王亚丽,萨日娜,等.不同生长期当归1H NMR指纹图谱的研究[J].波谱学杂志,2013,30(1):69-79.
[26]黄挺,张伟,全灿,等.定量核磁共振法研究进展[J].化学试剂,2012,34(4):327-332，341.
[27]刘红梅,张明贤,刘杨平,等.超临界CO2萃取白芷中香豆素类成分的工艺优化研究[J].中成药,2004(2):6-9.

相似文献/References:

[1]刘仁浪,蒋翼杰,江美彦,等.紫色土中氮肥、磷肥、钾肥配施对白芷产量及有效成分的影响[J].江苏农业学报,2023,(01):208.[doi:doi:10.3969/j.issn.1000-4440.2023.01.024]
　LIU Ren-lang,JIANG Yi-jie,JIANG Mei-yan,et al.Effects of combined application of nitrogen fertilizer, phosphorus fertilizer and potassium fertilizer on yield and active components of Angelica dahurica in purple soil[J].,2023,(04):208.[doi:doi:10.3969/j.issn.1000-4440.2023.01.024]

备注/Memo

备注/Memo:
收稿日期：2019-10-08基金项目：国家自然科学基金项目(31860102）；甘肃省自然科学基金项目(18JR3RA185)；甘肃农业大学引进人才专项(GSAU-RCZX201704）；甘肃农业大学学科建设基金项目(GSAU-XKJS-2018-086)；甘肃农业大学盛彤笙科技创新基金项目(GSAU-STS1737）作者简介：杨兰(1995-），女，甘肃天祝人，硕士研究生，从事中药分析研究。(Tel)15095423067；(E-mail)2281988971@qq.com通讯作者：李欠,(Tel)18194222519；(E-mail)liqian1984@gsau.edu.cn。邱黛玉，(Tel)13679467228；(E-mail)qiudy@gsau.edu.cn
更新日期/Last Update: 2020-09-08