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Extraction method for limonin

A technology of limonin and an extraction method, applied in the directions of steroids, organic chemistry, food science, etc., can solve the problems of high cost, high process cost, unfavorable industrial production of limonin, etc., and achieves easy operation and low process cost. Effect

Active Publication Date: 2014-08-27
罗达萌蒂(成都)生物医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using traditional methods, such methods are costly and time-consuming, which is not conducive to the industrial production of limonin, and part of limonin exists in aqueous solution in the form of limonin A cyclic lactone soluble, so it is difficult to separate
Some researchers use resin to adsorb limonin in aqueous solution, and then use organic solvent to elute the adsorbed limonin. This method also needs to use a large amount of organic solvent, and the organic solvent needs to be recovered, and the process cost is high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Step 1: The pomelo was squeezed to obtain an extract, and the content of limonin in the extract was determined to be 84.21 μg / mL.

[0025] Step 2, prepare ammonium sulfate solution with 80% saturation concentration; mix 1 mL of ammonium sulfate solution with 80% saturation concentration and 4 mL grapefruit extract evenly to obtain grapefruit with sulfate ion concentration of 0.85 mol / L and pH value of 4.17 extract.

[0026] Step 3: Heat at 50°C for 90 minutes, then heat at 100°C for 20 minutes.

[0027] Step 4: Centrifuge for 10 min at a rotational speed of 2500 × g.

[0028] The precipitate was redissolved with 4 mL of 60% acetonitrile, and its limonin content was determined to be 6.29 μg / mL. The calculated total limonin extraction rate was 7.47%.

Embodiment 2

[0030] Step 1: The pomelo was squeezed to obtain an extract, and the content of limonin in the extract was determined to be 85.87 μg / mL.

[0031] Step 2: Prepare a 100% saturated concentration of ammonium sulfate solution; mix 1 mL of 100% saturated concentration of ammonium sulfate solution with 4 mL of grapefruit extract evenly to obtain grapefruit with a sulfate ion concentration of 1.07 mol / L and a pH value of 4.14 extract.

[0032] Step 3: Heat at 50°C for 90 minutes, then heat at 100°C for 20 minutes.

[0033] Step 4: Centrifuge for 10 min at a rotational speed of 2500 × g.

[0034] The precipitate was redissolved with 4 mL of 60% acetonitrile, and the limonin content was determined to be 22.92 μg / mL, and the calculated limonin extraction rate was 26.69%.

[0035] Example 1 and Example 2 illustrate that the extraction rate of limonin is directly proportional to the concentration of ammonium sulfate in fruit juice.

Embodiment 3

[0037] Step 1. Soak pomelo directly in tap water to obtain an extract, adjust the pH of the pomelo extract to 4 with disodium hydrogen phosphate, and measure the limonin content in the extract to be 60.11 μg / mL.

[0038] Step 2: Prepare a 100% saturated concentration of ammonium sulfate solution; mix 1 mL of 100% saturated concentration of ammonium sulfate solution with 4 mL of grapefruit extract evenly to obtain grapefruit with a sulfate ion concentration of 1.07 mol / L and a pH value of 3.98 extract.

[0039] Step 3: Heat at 100 °C for 20 min.

[0040] Step 4: Centrifuge for 10 min at a rotational speed of 2500 × g.

[0041] The precipitate was redissolved with 4 mL of 60% acetonitrile, and the limonin content was determined to be 17.25 μg / mL, and the extraction rate of limonin was calculated to be 28.70%.

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Abstract

The invention discloses an extraction method for limonin. The extraction method includes the following steps of (1) raw material extracting in a soaked mode or juicing, wherein a raw material is directly soaked in water or directly juiced through a squeezer to obtain an extraction solution; (2) metal salt adding and pH adjusting, wherein sulfate solid matter or a sulfate saturated solution is added to the extraction solution, and the pH is adjusted to be 3-7; (3) heating and temperature keeping, wherein the solution is heated to 20 DEG C-100 DEG C, and the temperature is kept for 10 min-110 min; (4) centrifuging, the solution is centrifuged for 10 min at the rotating speed of 2500*g to obtain a limonin precipitate. Compared with a traditional method, the raw material can be directly soaked to obtain the extraction solution or directly juiced to obtain a squeezed solution without being dried by adopting the method, most of the limonin in the water is recovered through a precipitation method, complex equipment is not needed, and the extraction method is simple and convenient to operate and low in technological cost.

Description

technical field [0001] The invention relates to a method for extracting limonin, in particular to a method for extracting limonin by precipitation. Background technique [0002] Limonoid analogues are a class of highly oxidized tetracyclic triterpenoids mainly found in Rutaceae and Meliaceae plants. Since Bemay (1841) isolated limonin for the first time, people have successively isolated different limonin analogues. At present, more than 300 limonin analogues have been isolated from citrus plants and their hybrid plants. [0003] In recent decades, it has been found that limonoid analogues in citrus fruits have many biological functions: antimalarial, antibacterial, anti-inflammatory, analgesic, and insecticidal functions, which can effectively prevent pathogenic bacteria from invading the animal body, and can expel Parasites in animals; it can stimulate the activity of the main detoxifying enzyme in the body - glutathione transferase, and has strong anticancer activity; a ...

Claims

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Application Information

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IPC IPC(8): C07J73/00
CPCC07J73/008A23L27/2024A23L33/105A23V2002/00C07J73/00
Inventor 倪辉蔡慧农杨远帆高秋芬陈峰杜希萍黄高凌伍菱肖安风
Owner 罗达萌蒂(成都)生物医药科技有限公司
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