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Preparation method for nepetalactone

A technology of nepetalactone and refined liquid, which is applied in directions such as organic chemistry, can solve the problems of complicated operation steps, high cost, unsuitable for industrialized large-scale production and the like, and achieves the effects of high extraction rate, simple extraction process and low cost.

Inactive Publication Date: 2012-05-23
NANJING UNIVERSITY OF TRADITIONAL CHINESE MEDICINE
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Problems solved by technology

[0009] The problems and disadvantages of the above-mentioned nepetalactone extraction and refining method are that the operation steps are cumbersome, and the yield of nepetalactone is low. The whole process of nepetalactone takes about 7-8 weeks, and the yield is only 0.0161 %, the cost is high, not suitable for the needs of large-scale industrial production

Method used

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  • Preparation method for nepetalactone
  • Preparation method for nepetalactone
  • Preparation method for nepetalactone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] The extraction of embodiment 1 nepeta volatile oil

[0055] Take 25kg of the aerial part of Schizonepeta tenuifolia Briq., a plant of Labiatae, put it in a volatile oil extraction tank, add water to immerse the medicinal materials, set up the extraction device, steam distillation for 10 hours, and separate the oil and water to obtain 200 g of water-containing volatile oil of Schizonepeta. Freeze at -12°C for 24 hours, remove ice and water, and obtain 190 g of nepeta volatile oil.

Embodiment 2

[0056] The extraction of embodiment 2 nepeta volatile oil

[0057] Take 23.1 kg of flower spikes of Schizonepeta tenuifolia Briq., a Lamiaceae plant, put them in a volatile oil extraction tank, add water to immerse the medicinal materials, set up an extraction device, steam distillation for 10 hours, and separate the oil and water to obtain 231 g of water-containing Schizonepeta volatile oil. Freeze at -12°C for 24 hours, remove ice and water, and obtain 220 g of nepeta volatile oil.

Embodiment 3

[0058] The extraction of embodiment 3 nepeta volatile oil

[0059] Take 10kg of flower spikes of the Lamiaceae plant Schizonepeta tenuifolia Briq., put in CO 2 In the supercritical extraction device, the extraction pressure is 20MPa, the temperature is 45°C, and the CO 2 The flow rate is 2ml / g crude drug·min, the extraction time is 150min, and 220g of nepeta volatile oil is obtained.

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Abstract

The invention relates to a preparation method for nepetalactone, which has the characteristics of simple operation, high yield and low production cost. The method comprises the following steps of: A. introducing oxygen for oxidizing volatile oil of herba schizonepetae to obtain oxidized nepeta oil which is called reaction oil for short; B. performing silica gel column chromatography on the reaction oil obtained in the step A; degreasing by using petroleum ether solution which contains 5 to 15 percent of ethyl acetate; eluting by using the petroleum ether solution which contains 20 to 50 percent of the ethyl acetate to obtain an eluant; and recovering the eluant under a reduced pressure to obtain eluted refining liquid; and C. adding petroleum ether into the eluted refining liquid obtainedin the step B; refrigerating mixed liquid in a refrigerator; and obtaining the nepetalactone by crystallizing, ice-bathing and filtering. The preparation method for the nepetalactone has the characteristics of high yield and low production cost.

Description

technical field [0001] The invention relates to a method for preparing monoterpenoids, in particular to a method for preparing nepetalactone from natural raw materials. Background technique [0002] Nepetalactone is a monoterpenoid monomer compound extracted from the Chinese herbal medicine Schizonepetae. It is colorless crystals (ethyl acetate), mp: 188~189°C. TLC is red (10% ethanol sulfate), molecular formula is C 10 h 14 o 3 , its structural formula is as follows: [0003] [0004] Nepetalactone (C 10 h 14 o 3 , Schizonepetin) [0005] Schizonepeta tenuifolia Briq. is a Labiatae plant, which contains a large amount of volatile oil. The aerial parts or flower spikes are used as traditional Chinese medicine, and both have the effect of relieving exterior and dispersing wind. [0006] Schizonepeta volatile oil is the volatile oil extracted from the aerial parts or flower spikes of Schizonepeta tenuifolia Briq., which is commercially available. [0007] Chinese ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/83
Inventor 丁安伟张丽单鸣秋包贝华曹雨诞于生
Owner NANJING UNIVERSITY OF TRADITIONAL CHINESE MEDICINE
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