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Method for extracting limonin in lemon seeds by HPMC sedimentation assisted reversed micelles

A technology of limonin and lemon seeds, applied in the directions of steroids, organic chemistry, etc., can solve the problems of waste of limonin resources, adverse environmental effects, low extraction efficiency, etc., and achieve the level of promoting green development, easy promotion, and profit. high effect

Active Publication Date: 2018-09-07
重庆汇达生物科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Limonin in lemon fruit is mainly concentrated in lemon seeds, and is usually miscible with other fat-soluble components in the oil in lemon seed capsules. It is difficult to separate, and the extraction efficiency of conventional methods is low.
At present, lemon seeds or fragments in the process of lemon fruit processing are usually directly landfilled or incinerated as waste, which not only has a negative impact on the environment, but also causes a huge waste of limonin resources

Method used

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  • Method for extracting limonin in lemon seeds by HPMC sedimentation assisted reversed micelles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] (1) Drying and crushing of lemon grains or grain fragments: reduce the moisture content of lemon grains or grain fragments to less than 5% at 40°C, crush them with a grinder, and filter through a 150-200 mesh screen for later use.

[0043] (2) Rough extraction: add 0.1mmol / L citric acid-sodium citrate buffer (pH 6.6) to the lemon seed powder in step (1), adjust the ratio of liquid to material to 40:1~50:1, and then place Perform ultrasonic oscillation in an ultrasonic oscillator with an ultrasonic frequency of 40kHz (power 210W), a temperature of 40°C, and a time of 1-1.5h. Finally, it was placed at 4 °C for 10-12 h for later use.

[0044] (3) Initial Limonin Extract: Add HPMC powder with a mass fraction of 0.5% of the total mass to the crude extract prepared in step (2), and use a propeller-type stirrer to stir at a high speed to induce dissolution, and the stirring speed is 2000 r / min, time 0.5~1 h. Then, slowly add solid citric acid to adjust the pH to 5.5-6.0, st...

Embodiment 2

[0053] (1) Drying and crushing of lemon grains or grain fragments: reduce the moisture content of lemon grains or grain fragments to less than 5% at 40°C, crush them with a grinder, and filter through a 150-200 mesh screen for later use.

[0054] (2) Rough extraction: Add 0.1 mmol / L citric acid-sodium citrate buffer solution (pH 6.6) to the lemon seed powder in step (1), adjust the ratio of liquid to material to 40:1~50:1, and then place Ultrasonic oscillation was carried out in an ultrasonic oscillator with an ultrasonic frequency of 30kHz (power 180W), a temperature of 40-45°C, and a time of 2-3 h. Finally, it was placed at 4 °C for 10-12 h for later use.

[0055] (3) Initial Limonin Extract: Add HPMC powder with a mass fraction of 0.5% of the total mass to the crude extract prepared in step (2), and use a propeller-type stirrer to stir at a high speed to induce dissolution, and the stirring speed is 2000 r / min, time 0.5~1 h. Subsequently, slowly add tartaric acid to adju...

Embodiment 3

[0064] (1) Drying and crushing of lemon grains or grain fragments: reduce the moisture content of lemon grains or grain fragments to less than 5% at 40°C, crush them with a grinder, and filter through a 150-200 mesh screen for later use.

[0065] (2) Rough extraction: Add 0.1 mmol / L citric acid-sodium citrate buffer solution (pH 6.6) to the lemon seed powder in step (1), adjust the ratio of liquid to material to 40:1~50:1, and then place Perform ultrasonic oscillation in an ultrasonic oscillator, ultrasonic frequency 60kHz (power 240W), temperature 45~50℃, time 0.5~1.0h. Finally, it was placed at 4 °C for 10-12 h for later use.

[0066](3) Initial Limonin Extract: Add HPMC powder with a mass fraction of 0.5% of the total mass to the crude extract in step (2), and use a propeller-type stirrer to stir at a high speed to induce dissolution, and the stirring speed is 2000 r / min, time 0.5~1 h. Subsequently, slowly add fumaric acid to adjust the pH to 5.5-6.0, stir with a propell...

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Abstract

The invention provides a method for extracting limonin in lemon seeds by HPMC sedimentation assisted reversed micelles, and the method is used for extracting and preparing limonin in lemon grains or pieces of lemon grains. The method comprises the following steps: crushing raw materials; preparing a crude extracting solution; preparing a limonin primary extracting solution; preparing a reversed micelle extracting solution and a re-extraction water phase; performing pre-extraction on the reversed micelle extracting solution for the primary extracting solution, and separating out an upper-layerorganic phase; performing reversed extraction on the upper-layer organic phase through a reversed extraction water phase, and separating out a lower-layer water phase; hydrolyzing an acidic solution for the lower-layer water phase to prepare an acidolysis solution; and purifying the acidolysis solution to prepare limonin powder. The method for extracting limonin in lemon seeds by HPMC sedimentation assisted reversed micelles can sufficiently extract limonin in lemon peel residues, and is high in yield. The whole extracting method is simple in process, is low in cost, is beneficial for amplifying and performing industrial production; the method is simple and feasible, does not need a high-value complex apparatus, does not need professional training by a related operator, and is easily popularized.

Description

technical field [0001] The invention relates to a method for hydroxypropyl methylcellulose (HPMC) precipitation-assisted reverse micelles to extract limonin in lemon seeds, and belongs to the field of comprehensive utilization of by-products of fruit and vegetable processing and extraction of functional substances. Background technique [0002] Limonin (Limonin) is abundantly present in Rutaceae fruits such as citrus, lemon, pomelo, etc. It is a triterpene dilactone macromolecular compound that is electrically neutral and insoluble in water, but easily soluble in organic solvents such as chloroform, methanol, ethanol, isopropanol, acetonitrile, and acetone. Medical experiments in recent years have confirmed that limonin has strong antioxidant activity, can effectively maintain the balance of active oxygen free radicals in mammals, and at the same time inhibit the proliferation of cancer cells, delay arteriosclerosis, reduce cholesterol levels, dehumidify , analgesia, anti-i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J73/00
CPCC07J73/008
Inventor 汪开拓代领军张帮奎马莉伍冬志陈偲
Owner 重庆汇达生物科技股份有限公司
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