CN109731102B - Method for reducing anisidine value of olive oil - Google Patents

Method for reducing anisidine value of olive oil Download PDF

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CN109731102B
CN109731102B CN201910095411.6A CN201910095411A CN109731102B CN 109731102 B CN109731102 B CN 109731102B CN 201910095411 A CN201910095411 A CN 201910095411A CN 109731102 B CN109731102 B CN 109731102B
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olive oil
oil
stirring
reducing
anisidine value
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CN109731102A (en
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蔡鸿飞
潘裕清
许文东
杨阳
唐顺之
袁诚
龙海林
李海波
李康强
张懿
刘菊妍
蒋兆健
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Guangzhou Hanfang Pharmaceutical Co ltd
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Abstract

The invention relates to a method for reducing the anisidine value of olive oil, belonging to the technical field of refining and purifying the olive oil. The method for reducing the anisidine value of the olive oil comprises the following steps: (1) adding olive oil into a crystallization bottle, putting the bottle into a crystallization tank, and stirring at an initial crystallization temperature; (2) then cooling, and stirring and crystallizing at constant temperature; (3) removing the upper layer of the olive oil which is not crystallized and solidified to obtain the olive oil with the methoxyaniline value reduced. The method is simple and convenient to operate, does not introduce any chemical reagent or other exogenous substances, can effectively improve the safety and stability of the olive oil, has small influence on the fatty acid composition of the triglyceride of the olive oil, almost has no influence on the quality of the triglyceride of the olive oil, can ensure the safety of clinical medication, and is suitable for large-scale industrial production.

Description

Method for reducing anisidine value of olive oil
Technical Field
The invention relates to a method for reducing the anisidine value of olive oil, belonging to the technical field of refining and purifying the olive oil.
Background
Olive oil is a vegetable oil extracted from fresh olive fruit, and is an important component of the Mediterranean diet. The olive oil is rich in monounsaturated fatty acid (55-83 percent of oleic acid), squalene, polyphenol and vitamin, has the effects of resisting oxidation, regulating cholesterol, preventing cancers, beautifying, adjusting human physiological functions and the like, enjoys the reputation of 'vegetable oil queen', 'liquid gold' and the like, and is widely applied to the fields of cosmetics, health care products, medical drugs and the like. High-end fat emulsion preparations prepared by taking olive oil as a raw material, such as olive oil fat emulsion and various oil fat emulsions, are applied to clinic as a concentrated high-energy parenteral nutrient solution, provide energy and fatty acid nutrients necessary for organisms for patients who can not eat normally and have serious lack of nutrition, and have extremely high nutritional value and clinical application value. However, because olive oil contains a large amount of unsaturated fatty acids, secondary oxidation products such as aldehydes, ketones and quinones are inevitably generated in the processing and storage processes, and the oxidation products have the potential risks of destroying the normal physiological functions of the human body and promoting the occurrence and deterioration of diseases, so that the common olive oil cannot meet the medicinal requirements. Therefore, the medicinal olive oil has strict control on secondary oxidation products of aldehyde, ketone, quinone and the like, and common olive oil needs to be subjected to necessary treatment to reduce secondary oxides of aldehyde, ketone, quinone and the like so as to meet the medicinal requirements.
The content of secondary oxidation products such as aldehyde, ketone and quinones in the oil is generally represented by a anisidine value (also called anisidine value), and the higher the content of the secondary oxidation products, the higher the anisidine value, the higher the deterioration degree of the oil. Therefore, in order to ensure the oxidation stability of the grease, the content of such oxides needs to be reduced as much as possible to reduce the potential risk of damaging the normal physiological functions of the human body and the occurrence and deterioration of diseases.
The patent with publication number CN107746747 discloses a method for reducing peroxide value and anisidine value of polyunsaturated fatty acid, which takes unsaturated fatty acid oil as raw material, L-cysteine hydrochloride, sorbitol and phytic acid as reducing agent, and active carbon, silica gel, silica, vermiculite and zeolite as adsorbent, so as to achieve the purpose of reducing the anisidine value of unsaturated fatty acid. The method introduces exogenous chemical reagents, so that the quality of the oil cannot be guaranteed, and the oil has larger potential safety hazard if used as medicinal oil in clinic.
The patent with publication number CN103343048A discloses a method for reducing the anisidine value of high-content fish oil, which comprises the steps of firstly adsorbing fish oil with an adsorbent under the protection of inert gas, filtering the adsorbent, then performing molecular distillation treatment on the fish oil, and then adsorbing the fish oil with the adsorbent under the protection of inert gas for the second time, thereby reducing the anisidine value of the fish oil. The method uses a molecular distillation technology, the distillation process requires extremely high vacuum degree, the requirement on the tightness of materials is extremely strict, the equipment processing difficulty is high, the manufacturing cost is high, and the large-scale industrialization difficulty is high.
The patent with publication number of US7867538 adopts sodium borohydride to reduce the anisidine value of soybean oil, but also has the problem that the quality of oil cannot be ensured by introducing chemical reagents.
In addition, many documents report methods for reducing the anisidine Value of oil and fat, for example, MIYAGI Atsushi et al, in the document Reduction in Oxidation Index Value of Fish Oils Using Hydrophobic nonperous skin Process, can reduce the anisidine Value of Fish oil by 58-72% by Using a Hydrophobic Nonporous density film, but hexane needs to be introduced during the implementation of the method, which has a great influence on the oil and fat quality.
In view of the above, it is necessary to develop a technology for reducing the anisidine value of medicinal oil, which is suitable for large-scale industrial production and does not affect the quality of oil.
At present, the winterization technology is mainly used for dewaxing grease, reducing the content of saturated fatty acid in the grease, improving the cold resistance of the grease, and ensuring that the grease can still keep clear and transparent at low temperature, thereby ensuring that the quality and the state of the grease are not changed. For example, patent application No. CN201410002986.6 discloses a dewaxing process for corn oil; the patent with the application number of CN201510088911.9 discloses a winterization method for effectively preventing winterization oil of tea seeds from being turbid and improving the product quality of the winterization oil. In both patents, the oil and fat are treated by winterization technology, but the technology is only limited to dewaxing and the oil and fat saturation fatty acid content is reduced to prevent the oil and fat from being turbid at low temperature, and the technology for winterization is not used for reducing the anisidine value of the olive oil.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the method for reducing the anisidine value of the olive oil, the method is simple and convenient to operate, the safety and stability of the olive oil can be effectively improved, and the large-scale industrial production is easy to realize.
In order to achieve the purpose, the invention adopts the technical scheme that: a method for reducing the anisidine value of olive oil comprises the following steps:
(1) adding olive oil into a crystallization bottle, putting the bottle into a crystallization tank, and stirring at an initial crystallization temperature;
(2) then cooling, and stirring and crystallizing at constant temperature;
(3) removing the upper layer of the olive oil which is not crystallized and solidified to obtain the olive oil with the methoxyaniline value reduced.
As a preferred embodiment of the method for reducing the value of olive oil methoxybenzylamine according to the present invention, the specific operation of step (1) is: adding oleum Olivarum into a three-mouth crystallizing bottle, adding a thermometer and a mechanical stirring paddle, placing into a crystallizing tank, and stirring at initial crystallizing temperature.
As a preferred embodiment of the method for reducing the anisidine value of olive oil according to the present invention, the olive oil is at least one of extra virgin olive oil, medium virgin olive oil, virgin olive lamp oil, refined olive oil, mixed olive oil, and olive pomace oil.
In the preferred embodiment of the method for reducing the anisidine value of olive oil, in the step (1), the stirring speed is 30-60 r/min, and the stirring time is 0.5-3 h.
In a preferred embodiment of the method for reducing the anisidine value of olive oil according to the present invention, in the step (1), the initial crystallization temperature is 15 to 30 ℃.
In a preferred embodiment of the method for reducing the anisidine value of olive oil according to the present invention, in the step (2), the temperature reduction rate is 0.02 to 0.5 ℃/min.
As a preferred embodiment of the method for reducing the anisidine value of olive oil, in the step (2), the constant temperature is-10 to 2 ℃.
In the preferred embodiment of the method for reducing the anisidine value of olive oil according to the present invention, in the step (2), the stirring speed is 30 to 60r/min, and the stirring time is 1 to 72 hours.
Compared with the prior art, the invention has the beneficial effects that: the method is simple and convenient to operate, does not introduce any chemical reagent or other exogenous substances, can effectively improve the safety and stability of the olive oil, has small influence on the fatty acid composition of the triglyceride of the olive oil, almost has no influence on the quality of the triglyceride of the olive oil, can ensure the safety of clinical medication, and is suitable for large-scale industrial production.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
In the embodiment of the invention, the anisidine value of the olive oil is determined according to a method for detecting the anisidine value described in the national standard GBT 24304-2009, and the determination of the fatty acid content of the olive oil refers to the fourth part of the olive oil as a pharmaceutical adjuvant in the Chinese pharmacopoeia 2015 edition.
Example 1
A method for reducing the anisidine value of olive oil comprises the following steps:
(1) adding 2L of extra-grade virgin olive oil into a 3L three-mouth crystallization bottle, connecting a thermometer and a mechanical stirring paddle, putting into a crystallization tank, and stirring for 3h at 30r/min at the initial crystallization temperature of 15 ℃;
(2) then cooling to 2 ℃ at the speed of 0.02 ℃/min, and stirring and crystallizing for 72 hours at the constant temperature of 2 ℃ at the speed of 60 r/min;
(3) removing the upper layer of the olive oil which is not crystallized and solidified to obtain the olive oil with the methoxyaniline value reduced.
Example 2
A method for reducing the anisidine value of olive oil comprises the following steps:
(1) adding 2L of extra virgin olive oil into a 3L three-mouth crystallization bottle, connecting a thermometer and a mechanical stirring paddle, putting into a crystallization tank, and stirring at 60r/min for 0.5h at the initial crystallization temperature of 30 ℃;
(2) then cooling to-2 ℃ at the speed of 0.02 ℃/min, and stirring and crystallizing at the constant temperature of-2 ℃ at the speed of 30r/min for 3 h;
(3) removing the upper layer of the olive oil which is not crystallized and solidified to obtain the olive oil with the methoxyaniline value reduced.
Example 3
A method for reducing the anisidine value of olive oil comprises the following steps:
(1) adding 2L of extra-grade virgin olive oil into a 3L three-mouth crystallization bottle, connecting a thermometer and a mechanical stirring paddle, putting into a crystallization tank, and stirring for 2h at the initial crystallization temperature of 25 ℃ at 45 r/min;
(2) then cooling to-5 ℃ at the speed of 0.1 ℃/min, and stirring and crystallizing at 30r/min for 2.5h at the constant temperature of-5 ℃;
(3) removing the upper layer of the olive oil which is not crystallized and solidified to obtain the olive oil with the lowered anisidine value.
Example 4
A method for reducing the anisidine value of olive oil comprises the following steps:
(1) adding 2L of extra virgin olive oil into a 3L three-mouth crystallization bottle, connecting with a thermometer and a mechanical stirring paddle, placing into a crystallization tank, and stirring at an initial crystallization temperature of 30 ℃ at 60r/min for 0.5 h;
(2) then cooling to-10 ℃ at the speed of 0.5 ℃/min, and stirring and crystallizing at the constant temperature of-10 ℃ at the speed of 30r/min for 1 h;
(3) removing the upper layer of the olive oil which is not crystallized and solidified to obtain the olive oil with the methoxyaniline value reduced.
Example 5
A method for reducing the anisidine value of olive oil comprises the following steps:
(1) adding 2L of middle-grade virgin olive oil into a 3L three-mouth crystallization bottle, connecting a thermometer and a mechanical stirring paddle, putting into a crystallization tank, and stirring for 0.5h at an initial crystallization temperature of 30 ℃ at 60 r/min;
(2) then cooling to-2 ℃ at the speed of 0.02 ℃/min, and stirring and crystallizing at the constant temperature of-2 ℃ at the speed of 30r/min for 3 h;
(3) removing the upper layer of the olive oil which is not crystallized and solidified to obtain the olive oil with the methoxyaniline value reduced.
Example 6
A method for reducing the anisidine value of olive oil comprises the following steps:
(1) adding 2L of olive lamp oil as primary oil into a 3L three-mouth crystallization bottle, adding a thermometer and a mechanical stirring paddle, putting into a crystallization tank, and stirring at 60r/min for 0.5h at the initial crystallization temperature of 30 ℃;
(2) then cooling to-2 ℃ at the speed of 0.02 ℃/min, and stirring and crystallizing at the constant temperature of-2 ℃ at the speed of 30r/min for 3 h;
(3) removing the upper layer of the olive oil which is not crystallized and solidified to obtain the olive oil with the methoxyaniline value reduced.
Example 7
A method for reducing the anisidine value of olive oil comprises the following steps:
(1) adding 2L refined olive oil into a 3L three-mouth crystallization bottle, adding a thermometer and a mechanical stirring paddle, putting into a crystallization tank, and stirring at an initial crystallization temperature of 30 ℃ for 0.5h at a speed of 60 r/min;
(2) then cooling to-2 ℃ at the speed of 0.02 ℃/min, and stirring and crystallizing at the constant temperature of-2 ℃ at the speed of 30r/min for 3 h;
(3) removing the upper layer of the olive oil which is not crystallized and solidified to obtain the olive oil with the methoxyaniline value reduced.
Example 8
A method for reducing the anisidine value of olive oil comprises the following steps:
(1) adding 2L of mixed olive oil into a 3L three-mouth crystallization bottle, connecting a thermometer and a mechanical stirring paddle, putting into a crystallization tank, and stirring for 0.5h at an initial crystallization temperature of 30 ℃ at 60 r/min;
(2) then cooling to-2 ℃ at the speed of 0.02 ℃/min, and stirring and crystallizing at the constant temperature of-2 ℃ at the speed of 30r/min for 3 h;
(3) removing the upper layer of the olive oil which is not crystallized and solidified to obtain the olive oil with the methoxyaniline value reduced.
Example 9
A method for reducing the anisidine value of olive oil comprises the following steps:
(1) adding 2L of olive pomace oil into a 3L three-mouth crystallization bottle, connecting a thermometer and a mechanical stirring paddle, putting into a crystallization tank, and stirring for 0.5h at an initial crystallization temperature of 30 ℃ at 60 r/min;
(2) then cooling to-2 ℃ at the speed of 0.02 ℃/min, and stirring and crystallizing at the constant temperature of-2 ℃ at the speed of 30r/min for 3 h;
(3) removing the upper layer of the olive oil which is not crystallized and solidified to obtain the olive oil with the methoxyaniline value reduced.
Effect example 1
The special virgin olive oil, the medium virgin olive oil, the virgin olive lamp oil, the refined olive oil, the mixed olive oil and the olive pomace oil raw materials in the examples 1 to 9 mainly consist of fatty acid before treatment, indexes such as the anisidine value of the raw materials are shown in table 1, and the olive oil yield, the anisidine value and the main fatty acid composition after the treatment in the examples 1 to 9 are shown in table 2.
TABLE 1
Olive oil raw material Anisidine number Palmitic acid Stearic acid Oleic acid Linoleic acid
Extra virgin olive oil 8.4 13.304% 2.742% 70.202% 9.812%
Middle-grade virgin olive oil 13.2 12.531% 2.690% 69.898% 9.791%
Olive lamp oil for initial oil extraction 17.9 12.325% 2.793% 71.102% 9.690%
Refined olive oil 16.6 11.226% 2.593% 72.457% 10.109%
Mixed olive oil 12.4 12.432% 3.021% 69.578% 9.470%
Olive pomace oil 14.8 14.109% 2.841% 68.451% 10.795%
TABLE 2
Olive oil raw material Yield of Anisidine number Palmitic acid Stearic acid Oleic acid Linoleic acid
Example 1 Extra virgin olive oil 53.50% 4.5 13.329% 2.753% 70.107% 9.667%
Example 2 Extra virgin olive oil 69.76% 4.9 13.347% 2.766% 70.099% 9.597%
Example 3 Extra virgin olive oil 79.12% 5.4 13.251% 2.803% 70.021% 9.533%
Example 4 Extra virgin olive oil 73.89% 6.1 13.389% 2.811% 70.010% 9.523%
Example 5 Middle-grade virgin olive oil 75.10% 7.1 12.688% 2.702% 69.433% 9.690%
Example 6 Olive lamp oil for initial oil extraction 70.78% 9.2 12.401% 2.821% 71.003% 9.580%
Example 7 Refined olive oil 73.55% 8.4 11.487% 2.677% 72.153% 10.003%
Example 8 Mixed olive oil 68.09% 6.9 12.790% 3.109% 69.319% 9.379%
Example 9 Olive pomace oil 76.66% 8.0 14.189% 2.909% 68.198% 10.608%
As can be seen from tables 1 and 2, in examples 1 to 9, the method of the present invention can significantly reduce the anisidine value of olive oil, and the yield is high, and most importantly, the whole winterization process is completed at a low temperature, so as to ensure that the quality of olive oil is not changed. Meanwhile, because unsaturated fatty acids in the olive oil are mostly monounsaturated fatty acids, after winterization treatment, the content of each fatty acid component in the crystallized solid fat only slightly changes, and industrial large-scale production is easy to realize, which is significant when the olive oil is used as a pharmaceutic adjuvant. In conclusion, the method reduces the anisidine value of the olive oil by using winterization technology, and achieves the effect which cannot be achieved by other methods for reducing the anisidine value of the grease.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (2)

1. A method for reducing the anisidine value of olive oil is characterized by comprising the following steps:
(1) adding olive oil into a three-mouth crystallization bottle, connecting a thermometer and a mechanical stirring paddle, putting into a crystallization tank, and stirring at the initial crystallization temperature of 15-30 ℃; wherein the stirring speed is 30-60 r/min, and the stirring time is 0.5-3 h;
(2) then cooling at the speed of 0.02-0.5 ℃/min, and stirring at-10-2 ℃ for crystallization; wherein the stirring speed is 30-60 r/min, and the stirring time is 1-72 h;
(3) removing the upper layer of the olive oil which is not crystallized and solidified to obtain the olive oil with the methoxyaniline value reduced.
2. The method for reducing the anisidine value of olive oil according to claim 1, wherein the olive oil is at least one of extra virgin olive oil, medium virgin olive oil, virgin olive lamp oil, refined olive oil, mixed olive oil, olive pomace oil.
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CN111961527B (en) * 2020-09-03 2021-12-03 广州白云山汉方现代药业有限公司 Accurate control method for palmitic acid content in olive oil
CN113512466B (en) * 2021-07-16 2024-02-27 四川国为制药有限公司 Method for reducing peroxide value and methoxy aniline value in medicinal olive oil

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CN103710144B (en) * 2013-12-25 2015-03-25 南海油脂工业(赤湾)有限公司 Preparation method of low-methoxyaniline value soybean oil
WO2016007670A1 (en) * 2014-07-08 2016-01-14 Omega Protein Corporation Enrichment of palmitoleic acid palmitoleic acid derivatives by dry and solvent-aided winterization
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Application publication date: 20190510

Assignee: Guangyuan Rongshengyuan Food Co.,Ltd.

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