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

doi:10.3976/j.issn.1002-4026.2017.01.001

Abstract

Abstract:

The ¹H chemical-shift values of mollugin and purpurin in extract from Rubiae Radix et Rhizoma were assigned on the basis of 1D and 2D NMR, and a specific, simple, sensitive 1H NMR method has been developed and validated for the simultaneous quantitative determination of mollugin in extract from Rubiae Radix et Rhizoma When the solvent effects on the resolution of target signals and the solubility of the crude extracts were taken into account, dimethyl sulfoxide-d₆ was selected as an optimal ¹H NMR solvent. Quantitative determination was carried out by using the signal of the olefinic proton of mollugin (δ_H 5.77, H-2′) and H-3 of purpurin (δ_H 6.67), which were not interfere with other signals. Maleic acid was selected as internal standard because of its stable physical and chemical properties and having simple resonance signal. The improved method possessed good stability, repeatability, precision and accuracy for the quantification of mollugin and purpurin and the determination results agreed with the data obtained by HPLC-UV method. Due to its simple operation, short test time and without any reference

CLC Number:

R284.1

WANG Zhi-Wei, YAN Hui-Jiao, WANG Xiao, CHEN Yue, LIN Yun-Liang. Quantitative determination of mollugin and purpurin from traditional Chinese medicine Rubiae Radix et Rhizoma by ¹H NMR[J].SHANDONG SCIENCE, 2017, 30(1): 1-7.

References

［1］国家药典委员会.中华人民共和国药典2015年版一部［M］. 北京：中国医药科技出版社，2015: 234.
［2］ITOKAWA H, MIHARA K, TAKEYA K. Studies on a novel anthraquinone and its glycosides isolated from Rubiae Radix et Rhizoma and R. akane［J］. Chem Pharm Bull, 1983, 31(7): 2353-2358.
［3］ITOKAWA H, QIAO Y F, TAKEYA K, et al. New triterpenoids from Rubiae Radix et Rhizoma var. pratensis (Rubiaceae) ［J］. Chem Pharm Bull, 1989, 37(6): 1670-1672.
［4］CHUNG M I, JOU S J, CHENG T H, et al. Antiplatelet constituents of formosan Rubia akane［J］.J Nat Prod, 1994, 57(2): 313316.
［5］JEONG G S, LEE D S, KIM D C, et al.Neuroprotective and antiinflammatory effects of mollugin via upregulation of heme oxygenase-1 in mouse hippocampal and microglial cells［J］. Eur J Pharmacol, 2011, 654(3): 226-234.
［6］陈星, 王侃,单鸣秋,等.UPLC测定茜草炭中4种醌类成分的含量［J］.中国中药杂志, 2012, 37(19): 2922-2925.
［7］TANAKA R, NITTA A, NAGATSU A. Application of a quantitative ¹H-NMR method for the determination of amygdalin in Persicae semen, Armeniacae semen, and Mumefructus［J］.J Nat Med, 2014, 68(1): 225-230.
［8］HOHMANN M, FELBINGER C, CHRISTOPH N, et al. Quantification of taurine in energy drinks using 1H NMR［J］. J Pharm Biomed Anal, 2014, 93: 156-160.
［9］PIERI V, BELANCIC A, MORALES S, et al.Identification and quantification of major steviol glycosides in Stevia rebaudiana purified extracts by 1H NMR spectroscopy［J］. J Agric Food Chem, 2011, 59(9): 4378-4384.
［10］LI C Y, XU H X, HAN Q B, et al.Quality assessment of Radix Codonopsis by quantitative nuclear magnetic resonance［J］.Journal of Chromatography A, 2009, 1216(11): 2124-2129.
［11］WANG Z W, WANG J S, YANG M H, et al. Developmental changes in the composition of five anthraquinones from Rheum palmatum as quantified by 1HNMR［J］. Phytochem Anal, 2013, 24(4): 329-335.
［12］HOLZGRABE U.Quantitative NMR spectroscopy in pharmaceutical applications［J］. Prog Nucl Magn Reson Spectrosc, 2010, 57(2): 229-240.
［13］NAPOLITANO J G, GDECKE T, RODRGUEZBRASCO M F, et al.The tandem of full spin analysis and qHNMR for the quality control of botanicals exemplified with Ginkgo biloba［J］.J Nat Prod, 2012, 75(2): 238-248.
［14］PAULI G F, GDECKE T, JAKI B U, et al. Quantitative 1H NMR： Development and potential of an analytical method: An update［J］. J Nat Prod, 2012, 75 (4): 834-851.
［15］BURTON I W, QUILLIAM M A, WALTER J A. Quantitative 1H NMR with external standards: Use in preparation of calibration solutions for algal toxins and other natural products［J］. Anal Chem, 2005, 77(10): 3123-3131.

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Quantitative determination of mollugin and purpurin from traditional Chinese medicine Rubiae Radix et Rhizoma by ¹H NMR

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Quantitative determination of mollugin and purpurin from traditional Chinese medicine Rubiae Radix et Rhizoma by 1H NMR

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Quantitative determination of mollugin and purpurin from traditional Chinese medicine Rubiae Radix et Rhizoma by ¹H NMR