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14suitable and most easy to operate. Through the observation and analysis about the above cases, Shallow needling treatment and mild reinforcing reducing method are all effective and the shallow needling treatment is a superior therapy in the treatment of children facial neuritis. References
1 Songlin YU. Medlical Statistics[M]. Beijing: People's Medical Publishing House ,2002: 422, 341.
2 Qicai Wang. Subject of Acupuncture and Moxibustion Theraphy [M]. Beijing: China Press of traditional Chinese Medicine, 2004:87.
Three New Glycosides from the fruits of Xanthium sibirieum Patr.
Hui Hou, Hai Jiang, Liu Yang, Qiuhong Wang, Bingyou Yangand, HaixueKuang*
Key Laboratory of Chinese MateriaMedica, Ministry of Education, Heilongjiang University of
Chinese Medicine, Harbin 150040, P. R. China
Abstracts: Three new glycosides, named3p-norpinan-2-one-3-0-P-D-apiofuranosyl(1-6)P-D-glucopyranoside(1), 3-hydroxymethyl-7-methylocta-1,6-dien-3-ol-8-0-P-D-glucopyranoside (2), and 7-[P-D-apiofuranosyl-(1-6) P-D-glucopyranosyloxymethy]-8,8-dimethyl-4,8-dihydrobenzo [1,4]thiazine -3,5-dione(3), together with three known compounds, xanthiside (4), adenosine (5) and 2,3-dihydroxy-1-(4-hydroxy-3-methoxyphenyl)-propan-1-one (6) were isolated from the fruits of Xanthium sibiricumPatr..The structures of the new compounds were determined on the basis of detailed spectroscopic analyses.
Key words:XanthiumsibiricumPatr, Fruit, Glycosides
Fructusxanthii, the fruits of Xanthium sibiricumPatr.in the Compositae family, which is well known as Cangerzi, has been used for treating nasal sinusitis, numbness of the limbs, arthritis, ulcer, pruritus cancer and herpes [1-5] in traditonal medicine. Earlier chemical studies on F. xanthii led to the isolation of a series of essential oils, amino acid, organic acid, sesquiterpene lactones, diterpenes and thiazinedione [6-12]. In this article, we present the isolation and structure elucidation of three new compounds 3p-norpinan-2-one-3-0-P-D-apiofuranosyl(1-6)P-D-glucopyranoside(1), 3-hydroxymethyl-7-methylocta-1,6-dien-3-ol-8-O-P-D-glucopyranoside (2) and7-[p-D-apiofuranosyl-(1-6)P-D-glucopyranosyloxymethy]-8,8-dimethyl-4,8-dihydrobenzo [1,4]thiazine-3,5-dione (3), as well as three known compounds: xanthiside (4) [9], adenosine (5) [13], and 2,3-dihydroxy-1-(4-hydroxy-3-methoxyphenyl)-propan-1-one (6) [14] from the ethanol extract of the fruits of Xanthium sibiricumPatr..
Materials and methods
General:IR spectra were recorded on an IR-47 spectrometer. optical-rotation detector (Shodex OR-2, Showa Denko Co., Ltd. , Japan).The optical rotation was recorded on a Perkin-Elmer 241. The melting point was measured on Koflermicromelting point apparatus (uncorrected). The HRESIMS analyses were conducted on IonSpecUltima 7.0T FTICR. The UV and NMR spectra were recorded on SHIMADZU UV-1601 and Bruker DPX 400 (400 MHz for *H-NMR and 100
13
MHz for C-NMR), respectively. Chemical shifts are given as 5 values with reference to tetramethylsilane (TMS) as an internal standard, and coupling constants are given in Hz. Preparative HPLC (Waters, Delta 600-2487) was performed on Hypersil-ODS II column (10 ^m, 20x300 mm, Yilite, Da Lian, China). Silica gel (200-300 mesh, Yanghai, Qing Dao, China) and ODS-A (120 A, 50 ^m, YMC Co.) were employed for column chromatography (CC).
Plant material:The fruit of Xanthium sibiricum were collected from Hei Long Jiang Province of China in August in 2011, and authenticated by Prof. WANG Zhen-Yue of Heilongjiang University of Chinese Medicine. A voucher specimen (No. 20111077) is deposited at the Herbarium of Heilongjiang University of Chinese Medicine, Harbin, China.
Extraction and isolation: A 70% aqueous EtOH extract of the fruits ofXanthium sibiricum(2.7 Kg) was partitioned between EtOAc and H2O and between n-BuOH and H2O. The n-BuOH layers extract (59.4 g) was subjected to silica gel chromatography using CH2Cl2-MeOH mixtures (20:1, 10:1, 5:1, 2:1 v/v) to afford fractions A-D. Fr.A was stored. Fr.B(12.1g) was repeatedly subjected to ODS chromatography with MeOH-H2O (1:7-5:6) to afford compound 1 (9 mg) and 6 (24 mg). Fr.C (20.3g) was subjected to silica gel chromatography using CH2Cl2-MeOH mixtures (15:1, 5:1 v/v) to afford sub-fractions Ci and C2. Fr.C2 repeatedly was subjected to Sephadex LH-20 with CH2Cl2-MeOH (1:1), ODS with MeOH-H2O (2:1) and finally purified by preparative HPLC with MeOH-H2O(3:7) to afford compound 2 (3.2 mg). Fr.D (10.7g) was loaded on a Sephadex LH-20 column and eluted with CH2Cl2-MeOH (1:1) to yield five fractions, D1-D5. D2 (300 mg) was purified using semi-preparative HPLC with MeOH-H2O (2:3) to afford compound 3 (10.0 mg), compound 4 (19.0 mg) and compound 5 (57.1 mg). Conclusions
Through the extraction and separation,threenew glycosides, named3p-norpinan-2-one-3-0-P-D-apiofuranosyl(1-6)P-D-glucopyranoside(1), 3-hydroxymethyl-7-methylocta-1,6-dien-3-ol-8-0-P-D-glucopyranoside (2), and 7-[P-D-apiofuranosyl-(1-6) P-D-glucopyranosyloxymethy]-8,8-dimethyl-4,8-dihydrobenzo [1,4]thiazine -3,5-dione(3), together with three known compounds, xanthiside (4), adenosine (5) and 2,3-dihydroxy-1-(4-hydroxy-3-methoxyphenyl)-propan-1-one (6) were isolated from the fruits of Xanthium sibiricumPatr..The structures of the new compounds were determined on the basis of detailed spectroscopic analyses.This for later study on extraction and separation of Fructusxanthii provides certain reference conditions ; in the meantime For the toxicity of Fructusxanthii material research provides the corresponding structure analysis method. References
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Purification Process of Total jiegumuglycosides
LU Qing-xiu,Yang Liu, Jiang Hai,Wang Qiu-hong,Yang Bing-you, Kuang Hai-xue*
Key Laboratory of Chinese Materia Medica, Heilongjiang University of Chinese Medicine, Ministry of Education,Key Laboratory of Traditional Chinese Medicine and Natural Medicine Pharmacodynamic Material Base,Harbin 150040, China
Abstract: Objective To investigate the optimum parameters to purify total jiegumu glycosides. Method morroniside as index components,was established by HPLC analysis method morroniside determination; purification on total jiegumu glycosides has been studied. Result The purification process of total jiegumu glycosides is as following: the flow rate is 1.5BV/h, and themacroporous adsorptive resins is AB-8, then abandon 20BV eluant, gather 10% alcohol holo-elution. Conclusion Purification process is simple, reliable, and suitable for industrial production.
Key words: Sambucus williamsii Hance; morroniside; purification process
Sambucus williamsii Hance has a long history of medicinal,only contained in the "Tang Materia Medica",its root and root bark, stems and leaves, flowers were for medicinal. Alone used to
splice joints solid odd, then used drugs in the blood and blood, and its role in bone optimal ......
"exposition [1] Accoarding to the preliminary studies of task Force [2,3],The root of jiegumu have significantly promote fracture healing, and to clarify the material basis for total jiegumu glycosides[4]. Because of the research group of Sambucus williamsii Hance extraction process were studied. From the experiments can be seen, the dry extract in ethanol extracts morroniside (active ingredient) content of about 13.5%, and in order to achieve an effective component accounted for 50% of the effective parts. In this paper, morroniside as reference for the purification of total jiegumu glucosides study.
Materials and methods 1.1 Materials
Waters-2695 high performance liquid chromatography; electronic analytical balance (Switzerland METTLER TOLEDO Company); HPD-750, HPD-600, HPD-100 macroporous resin (Changzhou Bao En adsorption material Technology Co., Ltd.); AB-8 , D3520, S-8 macroporous resin (Nankai University chemical Plant); morroniside reference: Heilongjiang University of Chinese Medicine Department of Chemistry homemade (purity 98%), experimental herbs collected from Heilongjiang Province, East County, the Heilongjiang Chinese Medicine University School of
