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Method for extracting unsaponifiable matter from vegetable oil and application

An extraction method and technology for saponification, which are applied in the field of extraction of unsaponifiables of vegetable oil, can solve the problems of long extraction period, long time consumption, complicated separation and enrichment process, etc. Simple and effective extraction process

Active Publication Date: 2020-01-24
仕宝(天津)技术检测有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The extraction of unsaponifiable matter in the national standard method requires multiple extractions with organic solvents and multiple washings of the obtained organic phase until the pH reaches 7. Both will affect the extraction effect of unsaponifiable matter; the Chinese patent with the notification number CN101830770B discloses a method for extracting squalene from vegetable oil deodorization distillate, which specifically discloses the use of vegetable oil deodorization distillate as raw material, using The process of combining distillation, extraction and crystallization can extract high-concentration squalene, and simultaneously recover natural vitamin E and phytosterols with a certain purity; the Chinese patent with the notification number CN102565217B discloses a method for the simultaneous determination of phytosterols in vegetable oils. and the method of squalene, utilize dehydrated alcohol, potassium hydroxide solution and ascorbic acid solution to mix and make extracting solution in this method, extract the unsaponifiable matter wherein after boiling and refluxing, transfer saponified solution to and utilize ether to carry out cleaning separation after cooling solution, finally adding a small amount of ethanol or concentrated potassium hydroxide or sodium chloride solution for demulsification
In summary, the separation and enrichment process of unsaponifiables in vegetable oils is cumbersome and time-consuming. The unsaponifiables in vegetable oils obtained by existing methods will lose the unique advantages of fast analysis speed and simple sample preparation of infrared spectroscopy.

Method used

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  • Method for extracting unsaponifiable matter from vegetable oil and application
  • Method for extracting unsaponifiable matter from vegetable oil and application
  • Method for extracting unsaponifiable matter from vegetable oil and application

Examples

Experimental program
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Effect test

Embodiment 1

[0036] A method for extracting vegetable oil unsaponifiable matter, specifically comprising the following steps:

[0037] (1) Add 30mL of 2mol / L potassium hydroxide ethanol solution in 2g vegetable oil sample, vortex and shake for 0.5min, and carry out saponification process to it under ultrasonic heating; Wherein, ethanol in potassium hydroxide ethanol solution is Anhydrous ethanol;

[0038] (2) After the vegetable oil sample is saponified, add deionized water to the treatment solution and shake it up to dilute the saponified solution, then add n-hexane to extract the unsaponifiable matter; wherein, the added deionized water and n-hexane The volume ratio is 7:3, the amount of deionized water added is 35mL, and the amount of n-hexane added is 15mL. After extracting the unsaponifiable matter once, let it stand until the aqueous phase and the organic phase are separated, that is, the extraction of the unsaponifiable matter is completed;

[0039] (3) Design an SPE column special...

Embodiment 2

[0043] A method for extracting vegetable oil unsaponifiable matter, specifically comprising the following steps:

[0044] (1) Add 60mL of 2mol / L potassium hydroxide ethanol solution to 4g vegetable oil sample, vortex and shake for 0.7min, and carry out saponification treatment to it under the effect of ultrasonic heating; wherein, ethanol in potassium hydroxide ethanol solution is Anhydrous ethanol;

[0045] (2) After the vegetable oil sample is saponified, add deionized water to the treatment solution and shake it up to dilute the saponified solution, then add n-hexane to extract the unsaponifiable matter; wherein, the added deionized water and n-hexane The volume ratio is 7:3, the amount of deionized water added is 40mL, and the amount of n-hexane added is 18mL. After extracting the unsaponifiable matter once, let it stand until the aqueous phase and the organic phase are separated, that is, the extraction of the unsaponifiable matter is completed;

[0046] (3) Design an SP...

Embodiment 3

[0050] A method for extracting vegetable oil unsaponifiable matter, specifically comprising the following steps:

[0051] (1) Add 15mL of 2mol / L potassium hydroxide ethanol solution to 1g vegetable oil sample, vortex and shake for 0.6min, and carry out saponification treatment on it under the action of ultrasonic heating; wherein, ethanol in potassium hydroxide ethanol solution Anhydrous ethanol;

[0052] (2) After the vegetable oil sample is saponified, add deionized water to the treatment solution and shake it up to dilute the saponified solution, then add n-hexane to extract the unsaponifiable matter; wherein, the added deionized water and n-hexane The volume ratio is 7:3, the amount of deionized water added is 30mL, and the amount of n-hexane added is 12.8mL. After extracting the unsaponifiable matter once, let it stand until the aqueous phase and the organic phase are separated, that is, the extraction of the unsaponifiable matter is completed;

[0053] (3) Design an SPE...

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Abstract

The invention discloses a method for extracting unsaponifiable matter from vegetable oil, and the method specifically comprises the following steps of (1) adding a high-alkali saponification solutionto a vegetable oil sample for vortex shock for 0.5 to 0.7min and for subsequent saponification treatment under the effect of ultrasonic heating; (2) after the saponification treatment of the vegetableoil sample, firstly adding deionized water to a treatment solution for shaking to dilute, adding n-hexane to extract the unsaponifiable matter, leaving the treatment solution to stand after extracting the unsaponifiable matter once until the layering of an aqueous phase and an organic phase to complete the extraction of the unsaponifiable matter; (3) designing an SPE cartridge dedicated to waterand soap removal, and adsorbing the organic layer at the bottom after standing and layering to pass through the SPE cartridge for water and soap removal treatment, wherein the SPE cartridge is provided with a lower sieve plate, the lower layer is filled with 1 / 3 column volume of anhydrous sodium sulfate, and the upper layer is filled with 1 / 3 column volume of 3A molecular sieve; and (4) collectingthe effluent that passes through the SPE cartridge after water and soap removal in an evaporating dish, evaporating the solvent completely, and collecting infrared spectrums of the unsaponifiable matter for analysis.

Description

technical field [0001] The invention belongs to the technical field of oil detection and identification, and in particular relates to an extraction method and application of vegetable oil unsaponifiable matter. Background technique [0002] Vegetable oil is usually composed of saponifiable matter and unsaponifiable matter, among which, saponifiable matter accounts for 98.5%-99.5%, mainly various fatty acid glycerides, as many as hundreds of categories; unsaponifiable matter accounts for 0.5%-1.5% %, mainly including various phytosterols, tocopherols, squalene and pigments. The composition of edible vegetable oil is complex and the composition is very similar, therefore, it is difficult to screen out adulterated edible vegetable oil. [0003] In the existing vegetable oil identification or adulterated vegetable oil screening methods, there are mainly two categories: chromatography and spectrometry. Chromatography has the disadvantages of time-consuming sample preparation, c...

Claims

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Application Information

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IPC IPC(8): G01N21/35G01N21/3577G01N1/28
CPCG01N21/35G01N21/3577G01N1/28Y02W30/74
Inventor 何文绚卢先勇陈婷陈为健高仁金
Owner 仕宝(天津)技术检测有限公司
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