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Directional separation and purification method for diarylheptane-type compounds in saxifraga tangutica

A technology of diarylheptane and tanggut saxifrage is applied in the field of separation and purification of diarylheptane compounds to achieve the effect of easy scale expansion

Active Publication Date: 2018-12-25
CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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Problems solved by technology

Chinese patents CN 105153250B and CN 105085589A report the enrichment method of diaryl heptane compounds in Saxifrage tangutica and the diaryl heptane compounds with new structure and anti-tumor activity. Efficient purification methods for directional acquisition of diarylheptanes from earwort have not been reported in the literature

Method used

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  • Directional separation and purification method for diarylheptane-type compounds in saxifraga tangutica
  • Directional separation and purification method for diarylheptane-type compounds in saxifraga tangutica
  • Directional separation and purification method for diarylheptane-type compounds in saxifraga tangutica

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Embodiment

[0035] Select 95% ethanol extract of Saxifrage tangutica and extract fraction 7 obtained by MCI through ethyl acetate extraction. Three representative fractions (Fr2, Fr3 and F6) obtained by the first dimension preparation were obtained by the second dimension reversed-phase chromatography 8 diaryl heptane monomers. The structural information of the compound is shown in Table 1:

[0036] Table 1 7 diaryl heptane monomers

[0037]

[0038]

[0039] The specific process is as follows:

[0040]①Choose Fraction 2 and use the reversed-phase chromatographic separation mode for the second-dimensional preparative high-performance liquid chromatographic separation. Chromatographic conditions: the chromatographic column is resistant to pure water (XAqua C18, 250×20mm, i.d., 10μm); 0.2% formic acid-water (A) and acetonitrile (B) mobile phase system; 0~60min, volume concentration 25%→55%B gradient elution; Flow velocity is 15mL / min; Detection wavelength is 281nm; Collect two chrom...

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Abstract

The invention discloses a directional separation and purification method for diarylheptane-type compounds in saxifraga tangutica. Diarylheptane-type compound monomers are obtained by a medium-pressurechromatographic tower and a two-dimensional preparative liquid chromatography system. The directional separation and purification method has the advantages that the medium-pressure chromatographic tower and the two-dimensional preparative liquid chromatography are used for separating and purifying the diarylheptane-type compounds from ethyl acetate extraction portions of 95% ethanol extract of the saxifraga tangutica, wherein an MCI stationary phase is applied to the medium-pressure chromatographic tower, a hydrophilic chromatographic column (used in a normal phase system) is applied to first-dimension chromatographic separation, and a reversed-phase chromatographic column is applied to second-dimension chromatographic separation; the three-step chromatographic separation is operated visually, fast, simple, and easy to scale up and expand; by the method, target preparation of the diarylheptane-type compounds can be realized, known active diarylheptane can be obtained in batch, and trace diarylheptane can be enriched and separated, so that a diarylheptane-type compound library can be enriched continuously.

Description

technical field [0001] The invention relates to the technical field of separation and purification of diaryl heptane compounds, in particular to a method for the directional separation and purification of diaryl heptane compounds in Saxifrage tangutata. Background technique [0002] Saxifraga tangutica Engl. is a plant of the genus Saxifraga in the family Saxifragaceae. Its Tibetan medicine name is Songjidi, and it is called Diida in traditional Chinese medicine. It is mainly distributed in Qinghai, Gansu, Under the coniferous forest shrubs in Tibet, Sichuan, Bhutan and Kashmir at an altitude of 2900-4900m. Tangutia saxifrage is a commonly used Tibetan medicine. It tastes bitter and cool, clears away heat, treats liver, gallbladder fever and trauma, and can also treat acute otitis media and wind-heat cough. Modern pharmacological studies have shown that Tangutia saxifrage has antibacterial , antiviral, anti-inflammatory and anti-tumor pharmacological effects. [0003] So f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/79C07C49/255C07C49/248
CPCC07C45/79C07C49/248C07C49/255
Inventor 党军陶燕铎邵赟王启兰梅丽娟
Owner CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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