定量核磁共振氢谱法同时测定千年健中芳樟醇、原儿茶酸的含量<sup>*</sup>

蒋丽娟, 韦佳先, 周平秀, 张凤兰, 张夏雯, 李业航

doi:10.16155/j.0254-1793.2024.06.04

药物分析杂志 >

2024 , Vol. 44 >Issue 6: 946 - 951

DOI: https://doi.org/10.16155/j.0254-1793.2024.06.04

成分分析

定量核磁共振氢谱法同时测定千年健中芳樟醇、原儿茶酸的含量^*

展开

1.广西民族大学化学化工学院,广西多糖材料与改性重点实验室,广西高校化学与生物转化过程新技术重点实验室,南宁 530006;
2.广西民族大学医院,南宁 530006

第一作者 Tel:13152671318;E-mail:jianglj12@yeah.net

收稿日期: 2023-10-25

网络出版日期: 2024-08-07

基金资助

* 广西民族大学2023年实验技术创新与实验室管理研究项目(2023MDSY003)

收起

Simultaneous determination of linalool and protocatechuate in Homalomena occulta by quantitative nuclear magnetic resonance (qNMR) spectroscopy^*

Expand

1. School of Chemistry and Chemical Engineering, Guangxi Minzu University, Guangxi Key Laboratory for Polysaccharide Materials and Modification, Guangxi Higher Education Institutes Key Laboratory for New Chemical and Biological Transformation Process Technology, Nanning 5300, China;
2. Guangxi Minzu University Hospital, Nanning 5300, China

Received date: 2023-10-25

Online published: 2024-08-07

Fold

摘要

目的: 采用氢核磁定量方法快速测定千年健中主要成分芳樟醇、原儿茶酸的含量。方法: 以氘代二甲基亚砜为测试溶剂,吡嗪为内标物,在400 MHz光谱仪上进行¹H-qNMR测量,其中吡嗪、芳樟醇、原儿茶酸的定量共振峰分别为δ 8.66、δ 5.85~5.95、δ 6.78~6.80。结果: 芳樟醇、原儿茶酸的线性关系良好,相关系数分别为0.999 7、0.998 5,精密度RSD分别为0.30%、0.40%,回收率分别为98.8%~100.7%(RSD为3.7%)和99.4%~100.6%(RSD为4.4%),表明所建立的氢核磁定量方法,结果准确,稳定可行,且整个检测过程在3 min左右完成。4批千年健药材中芳樟醇、原儿茶酸的含量范围分别为0.328~0.398 mg·g^-1、0.559~0.630 mg·g^-1。结论: 该方法操作简单,分析速度快,专属性强,可用于千年健中2个有效成分的同步测定,为千年健药材的全面质量评价和质量控制提供科学依据。

关键词： 千年健; 芳樟醇; 原儿茶酸; 氢核磁共振; 多指标; 质量评价

本文引用格式

蒋丽娟, 韦佳先, 周平秀, 张凤兰, 张夏雯, 李业航 . 定量核磁共振氢谱法同时测定千年健中芳樟醇、原儿茶酸的含量^*[J]. 药物分析杂志, 2024 , 44(6) : 946 -951 . DOI: 10.16155/j.0254-1793.2024.06.04

Abstract

Objective: To establish a hydrogen nuclear magnetic quantitative method which can rapidly determine the contents of linalool and protocatechuate in Homalomena occulta. Methods: Using dimethyl sulfoxide-d₆(DMSO-d₆)as the test solvent and pyrazine -as the internal standard, ¹H-q NMR measurement was performed on a 400 MHz spectrometer. The quantitative resonance peaks of pyrazine, Linalool and protocatechuate were δ 8.66, δ 5.90 and δ 8.60, respectively. Results: The linear correlation coefficients of linalool and protocatechuate were good with r of 0.999 7 and 0.998 6, respectively. The RSDs of precision were 0.30% and 0.40%, and the recoveries were 98.8%-100.7%(RSD=3.7%) and 99.4%-100.6%(RSD=4.4%), respectively, which indicated that the established method was accurate, stable and feasible. And the whole detection process was completed in about three minutes. The contents of 2 components in 4 batches of Homalomena occulta were 0.328-0.398 mg·g^-1(linalool)and 0.559-0.630 mg·g^-1 (protocatechuate), respectively. Conclusion: The ¹H-q NMR method has the advantages of simple operation, fast analysis speed and specificity, and can be used for the simultaneous determination of two active components in Homalomena occulta, providing a scientific basis for the overall quality evaluation and quality control of Homalomena occulta.

Key words： Homalomena occulta; linalool; protocatechuate; ¹H-qNMR; multi-index; quantitative evaluation

参考文献

[1] 中华人民共和国药典2020年版.一部[S]. 2020: 34
ChP 2020. Vol Ⅰ[S]. 2020: 34
[2] 谢丽莎,龚志强,李娉. 千年健研究进展[J]. 上海中医药杂志,2015,45(11): 90
XIE LS, GONG ZQ, LI P. Advances in Homalomena occulta research[J]. Shanghai J Tradit Chin Med, 2015,45(11): 90
[3] 胡永美,杨中林,叶文才,等. 千年健化学成分的研究(I) [J]. 中国中药杂志,2003,28(4):342
HU YM, YANG ZL, YE WC, et al. Studies on the constituents in Rhizome of Homalomena occuta(Ⅰ) [J]. China J Chin Mater Med, 2003,28(4):342
[4] 胡永美, 杨中林, 叶文才,等.千年健化学成分研究(Ⅱ) [J]. 中成药,2006, 28(12):1794
HU YM, YANG ZL, YE WC, et al. Studies onthe constituents in Rhizome of Homalomena occuta(Ⅱ) [J]. Chin Tradit Pat Med,2006, 28(12):1794
[5] 张珍珍,李晋奇,曾明辉.千年健化学成分及其药理作用研究进展[J]. 成都中医药大学学报,2021,12.44(4): 98
ZHANG ZZ, LI JQ, ZENG MH. Advances in research on cheenical compositionand and pharmacological effects of Homalomena occulta[J]. J Chengdu Univ Tradit Chin Med, 2021, 12.44(4): 98
[6] 杨再波, 赵超.固相微萃取/气相色谱/质谱法分析千年健中挥发性化学成分[J]. 精细化工,2007,24(2): 149
YANG ZB, ZHAO C. Analysis of chemical constituents of the essential oil from Homalomena occulta schott by SPME-GC-MS[J]. Fin Chem Cals, 2007, 24(2): 149
[7] 茅银燕,岳显可. 基于主成分分析的不同产地千年健GC指纹图谱研究[J]. 药学研究,2017, 20(8): 933
MAO YY, YUE XK. GC fingerprint combined with principal component analysis in the study for Homalomena occulta from different habitats[J]. Pract Pharm Clin Remed, 2017, 20(8): 933
[8] 谢丽莎,蒙田秀,欧阳炜,等. GC法测定广西千年健芳樟醇的含量[J]. 中国药师,2012,12(5): 607
XIE LS, MENG TX, OUYANG W, et al. Determinnation of Linalool in Homalomona occulta from Guangxi by GC[J]. China Pharm, 2012,12(5): 607
[9] 佘金明,刘冰,王宪庆,等. HELP与GC-MS法分析千年健挥发油成分[J]. 中药材,2010,33(9):1421
SHE JM, LIU B, WANG XQ, et al. Analysis of the volatile oil components of Qianqianjian by HELP and GC-MS methods[J]. J Chin Med Mater, 2010,33(9):1421
[10] 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,2020,36(4): 1049
YANG L,LI Q,FENG YM, et al. Determination of imperatorin in Angelica dahuricae by quantitative nuclear magnetic resonance(qNMR)spectroscopy[J]. Jiangsu J Agric Sci, 2020, 36(4): 1049
[11] 范悦,李欠,常宝勤.定量核磁共振波谱法测定黄芩中的黄芩苷含量研究[J]. 中国野生植物资源,2022,41(3): 25
FAN Y,LI Q,CHANG BQ. Determination of baicalin in Scutellariae Radix by quantitative nuclear magnetic resonance spectroscopy[J]. Chin Wild Plant Res, 2022,41(3): 25
[12] 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, 43(1): 69
YU S,GUO QS,WANG HL, et al. Simultaneous Determination of resveratrol and polydatin in Polygonum cuspidatum by quantitative nuclear magnetic resonance spectroscopy[J]. Chin J Anal Chem, 2015, 43(1): 69
[13] 马秀琴,张瑜,冯彦梅,等,定量核磁共振波谱法测定川芎中藁本内酯含量[J]. 中兽医医药杂志,2020,39(4):59
MA XQ, ZHANG Y, FENG YM, et al. A validated 1^H-qNMR method for direct quantification of ligustilde in Ligusticum chuanxiong Hort[J]. J Tradit Chin Veter Med, 2020, 39(4):59
[14] 郭强胜,刘明珂,禹珊,等. 定量核磁共振法同时测定复合维生素B 片中B₁、B₂、烟酰胺和泛酸钙[J]. 波谱学杂志,2016,33(3):442
GUO QS, LIU MK, YU S, et al. A Quantitative NMR method to analyze vitamin B₁, vitamin B₂, nicotinamide and calcium pantothenate contents in compound vitamin B tablets[J]. Chin J Magn Resonance, 2016,33(3):442
[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
LIN S,SU J,YE J, et al. Application progress in quantitative NMR in analysis of traditional Chinese medicine[J]. J Pharm Pract, 2014,32 (2): 92
[16] 张芬芬,蒋孟虹,沈文斌,等.定量核磁共振(QNMR) 技术及其在药学领域的应用进展[J]. 南京师范大学学报(工程技术版), 2014,14(2): 8
ZHANG FF, JIANG MH, SHEN WB, et al. Progress in quantitative nuclear magnetic resonance technology in pharmaceutical applications[J]. J Nanjing Norm Univ (Eng Technol Ed), 2014, 14(2): 8
[17] 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
WANG ZW,YIN HJ,CHEN Y, et al. Simultaneous determination of emodin and physcion in Polygonum multiflorum by quantitative ¹H NMR[J]. Chin J Pharm Anal,2016,36(12): 2163
[18] KLYS A, OLSZEWSKA MA. A validated ¹H qNMR method for direct and simultaneous quantification of esculin,fraxin and(-)-epicatechin in Hippocastani cortex[J]. Talanta, 2019, 192:263

Options

文章导航

模态框（Modal）标题

摘要

本文引用格式

Abstract

参考文献