Pharmaceutical composition comprising an extract of pseudolysimachion longifolium and the catalpol derivatives isolated therefrom having antiinflammatory, antiallergic and antiasthmatic activity
A technology for allergic diseases and inflammatory diseases, which is applied in the fields of application, drug combination, and pharmaceutical formulation, and can solve problems such as the lack of reported or disclosed inhibitory effects of catalpol derivatives
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Embodiment 1
[0066] The preparation of the crude extract of embodiment 1. long leaf panicle
[0067] [0061] 7.9 kg of dried Acarina longifolia was cut into small pieces, mixed with 50 L of methanol, the mixture was stirred at room temperature for 24 hours, and extracted three times with cold water. The extract was filtered with filter paper to remove residue. The filtrate was pooled and concentrated by a rotary evaporator at 55-65° C. under reduced pressure and dried with a freeze dryer to obtain 950.5 g of dry crude extract of Pachyphylla longifolia.
Embodiment 2
[0068] The preparation of embodiment 2. polar solvent and non-polar solvent soluble extract
[0069] [0063] 2-1. Preparation of ethyl acetate soluble fraction
[0070] [0064] Add 10L distilled water to the crude extract obtained in 425g embodiment 1. 1.10 L of ethyl acetate was added thereto through a separatory funnel, and vigorously shaken to separate into an ethyl acetate-soluble layer and a water-soluble layer.
[0071] [0065] The above ethyl acetate soluble layer was concentrated with a rotary evaporator, and dried with a freeze dryer to obtain an ethyl acetate soluble extract.
[0072] [0066] 2-2. Preparation of butanol / water-soluble fraction
[0073] [0067] The water-soluble layer was fractionated by mixing with 10 L of butanol, and finally 144.0 g of n-butanol-soluble extract and water-soluble extract were obtained to be used as samples for the following experiments.
Embodiment 3
[0074] [0068] Example 3. Catalpol derivatives are prepared from the long leaf panicle flower extract
[0075] [0069] 3-1. Preparation of verbascoside (6-O-3,4-dihydroxybenzoyl catalpol)
[0076] [0070] 140.0g n-butanol soluble extract is carried out to silica gel column chromatography (70-230 mesh, 8.5 × 65cm), and eluted with chloroform-methanol mixture (methanol 0-100%, step gradient) to obtain five distillate. Using normal phase silica gel column chromatography (silica gel, 230-400 mesh, 6.0 × 60cm, chloroform-methanol mixture, methanol 10-50% step gradient) to 29.1g fraction 2 (in chloroform-methanol 7 / 3-6 / 4 Between, v / v) carry out repeated column chromatography. Fractions 2-4 were recrystallized from methanol to obtain 14.2 g of verbascoside, 6-O-3,4-dihydroxybenzoyl catalpol. By NMR ( 1 H, 13 C, DEPT, HMQC, HMBC), EI-MS and polarimetry and previously reported methods (Afifi-Yazar F et al., HeIv ChimActa, 63, 1905-7 pages, 1980) confirmed the structure, and the purit...
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