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Method for adsorbing and separating squalene from vegetable oil deodorized distillate

A deodorizing distillate, adsorption separation technology, applied in adsorption purification/separation, chemical instruments and methods, distillation purification/separation, etc., can solve the problems of inability to achieve high content, high cost, high cost, etc., and achieve a good choice The effect of strong adsorption and desorption, low recovery cost and good mechanical strength

Inactive Publication Date: 2016-09-21
HUIZHOU RES INST OF SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Posada et al. used molecular distillation technology to extract squalene from palm oil, and investigated the effects of distillation temperature and feed rate on the content of squalene in palm oil. The results showed that squalene can enter the light phase at low temperature Among them, the content is 3.94%, which has certain guiding significance for the extraction of squalene by molecular distillation (Separation and Purification Technology 2007, the second phase 220-229 pages). Although the processing capacity is large, the energy consumption is too large, the cost is too high, and the purity lower
Gunawan et al. studied the separation of squalene from soybean deodorization distillate through improved silica gel column chromatography. Compared with traditional silica gel column chromatography, it has the characteristics of saving solvent and short time consumption (Separation and Purification Reviews 2009 No. pp. 207-241 of the third issue), but this method is expensive and complicated to operate
The above-mentioned articles are all researches on their respective methods, and are limited in their respective deficiencies, especially in the preparation of high-purity squalene, which few technologies can achieve, even column chromatography technology cannot achieve high content (more than 95%), and the processing capacity is small, and the purification efficiency is not high
[0005] Adsorption method is widely used in the field of extraction and purification of natural active products, but there are few reports on the targeted adsorption of squalene in vegetable oil deodorization distillate, and the adsorption method has the advantages of reusability, simple operation, low cost and environmental protection. Therefore, the application of adsorption method to the extraction and purification of squalene is in line with the green and high-efficiency theme advocated by the environmental engineering field in recent years.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Weigh 0.20 g of D101 macroporous adsorption resin, put it into 50 mL of 2000 mg / L squalene olive oil deodorization distillate solution, place it in a full-temperature air bath at 20 °C and shake at a speed of 200 rpm / min Shake the shaker for 24 h. After the shaking, take the supernatant and use high-performance liquid chromatography to measure the content of squalene in the solution (4.6 mm×160 mm, 5 um, XDB-C18 chromatographic column, the mobile phase is methanol, the flow rate 1 ml / min, injection volume 10 um, detection wavelength 210 nm, column temperature 30°C), the results show that the adsorption capacity of the adsorbent for squalene is 165 mg / g. The adsorption material adsorbed with squalene was added to the n-hexane organic solvent for stirring and elution at room temperature, and the content of squalene in the solution was measured by high performance liquid chromatography. The result showed that the elution rate was 96%.

Embodiment 2

[0028] Weigh 0.20 g of D101 macroporous adsorption resin, put it into 50 mL of 1000 mg / L squalene soybean oil deodorization distillate solution, place it in a full-temperature air bath at 20 °C and shake at a speed of 200 rpm / min Shake the shaker for 24 h. After the shaking, take the supernatant and use high-performance liquid chromatography to measure the content of squalene in the solution (4.6 mm×160 mm, 5 um, XDB-C18 chromatographic column, the mobile phase is methanol, the flow rate 1 ml / min, injection volume 10 um, detection wavelength 210 nm, column temperature 30°C), the results show that the adsorption capacity of the adsorbent for squalene is 149 mg / g. The adsorption material adsorbed with squalene was added to diethyl ether for stirring and elution at room temperature, and the content of squalene in the solution was measured by high performance liquid chromatography, and the elution rate was 98%.

Embodiment 3

[0030] Weigh 0.20 g of D101 macroporous adsorption resin, put it into 50 mL of 1000 mg / L squalene cottonseed oil deodorization distillate solution, place it in a full-temperature air bath at 40 °C and shake at a speed of 200 rpm / min Shake the shaker for 24 h. After the shaking, take the supernatant and use high performance liquid chromatography to measure the content of squalene in the solution (4.6 mm×160 mm, 5 um, XDB-C18 chromatographic column, the mobile phase is methanol, the flow rate 1 ml / min, injection volume 10 um, detection wavelength 210 nm, column temperature 30°C), the results show that the adsorption capacity of the adsorbent for squalene is 118 mg / g. The adsorption material adsorbed with squalene was added to acetone for stirring and elution at room temperature, and the content of squalene in the solution was measured by high performance liquid chromatography. The result showed that the elution rate was 98%.

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Abstract

The invention discloses a method for adsorbing and separating squalene from vegetable oil deodorized distillate. According to the method for adsorbing and separating the squalene from the vegetable oil deodorized distillate provided by the invention, D101 type macroporous resin is used as an adsorbent. According to the method, an adsorbing material is directly thrown into a solution containing the squalene, and an efficient adsorption process can be completed at normal temperature. According to the method, organic solvents such as n-hexane are used for desorption, the desorption efficiency is extremely high, and the squalene can be efficiently purified. The adopted adsorbing materials do not dissolve in acid, alkali and the organic solvents, are excellent in mechanic strength, can be used repeatedly, is simple in regeneration technology, and low in reclamation cost. The adopted adsorbing materials statically and dynamically adsorb the squalene in the vegetable oil deodorized distillate at normal temperature, are excellent in preferential adsorption and desorption effects, and basically has no change in adsorbing capacity when being reused after desorption activation.

Description

technical field [0001] The invention belongs to the technical field of squalene extraction, and in particular relates to a method for adsorbing and separating squalene in vegetable oil deodorization distillates. Background technique [0002] Squalene is also known as squalene, tricosahexaene, and squalene, and its chemical name is 2,6,10,15,19,23-hexamethyl-2,6,10,14,18,22-twenty Tetracarbahexaene, molecular formula C 30 h 50 , with a molecular weight of 410.71, is a highly unsaturated hydrocarbon compound originally discovered in black shark liver oil by Japanese chemist Tsujimoto in 1906. Squalene is a natural triterpene, a polyunsaturated aliphatic hydrocarbon compound containing six non-conjugated double bonds. Squalene has significant antioxidant capacity, can inhibit the formation of cancer cells, and to a certain extent can prevent the proliferation of cancer cells and leukopenia due to chemotherapy, and has obvious curative effects on gastric cancer, esophageal ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C7/00C07C7/04C07C7/12C07C11/21
CPCC07C7/00C07C7/04C07C7/12C07C11/21
Inventor 纪红兵杨祖金李海波
Owner HUIZHOU RES INST OF SUN YAT SEN UNIV
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