CN110760385A - Method for removing benzopyrene in tea oil - Google Patents
Method for removing benzopyrene in tea oil Download PDFInfo
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- CN110760385A CN110760385A CN201911117997.8A CN201911117997A CN110760385A CN 110760385 A CN110760385 A CN 110760385A CN 201911117997 A CN201911117997 A CN 201911117997A CN 110760385 A CN110760385 A CN 110760385A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/10—Refining fats or fatty oils by adsorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
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- Chemical Kinetics & Catalysis (AREA)
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- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
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- Dispersion Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention belongs to the technical field of food processing, and particularly relates to a method for removing benzopyrene in tea oil. The invention comprises the following steps: (1) preparing montmorillonite hydrothermal carbon composite material; (2) adding untreated tea oil; (3) centrifuging and standing; (4) freezing and layering; (5) and (5) separating the benzopyrene. The separation material used in the invention is the montmorillonite hydrothermal carbon composite material, which does not have qualitative change chemical reaction with the tea oil and the benzopyrene, has no influence on the quality of the tea oil, does not destroy beneficial components in the tea oil, and does not cause the loss of the tea oil. Meanwhile, new harmful residues cannot be introduced to cause secondary pollution in the tea oil, the removal efficiency of the benzopyrene is high and can reach more than 90%, and the content of the benzopyrene in the treated tea oil sample can reach below the specified range of GB 2716-2005 edible vegetable oil health Standard. The method has the advantages of simple operation, short reaction time, safety, effectiveness, economy and environmental protection.
Description
Technical Field
The invention belongs to the technical field of food processing, and particularly relates to a method for removing benzopyrene in tea oil.
Background
The tea oil is obtained from seeds of Camellia oleifera in Theaceae, called Camellia oleifera seed oil and Camellia oil, and is a unique edible oil of woody plant in China. The content of unsaturated fatty acid in the tea oil is up to 90 percent, wherein the oleic acid is 75 to 83 percent, the linoleic acid is 7.4 to 13 percent, the tea oil is very similar to the olive oil which is the best woody edible vegetable oil recognized in the world, and is called as the oriental olive oil. The tea oil contains various functional components, and has obvious effects of maintaining the functions of cardiovascular systems, improving the immunity of human bodies, reducing cholesterol and preventing and treating hypertension. In addition, the traditional medicine believes that the tea oil has the functions of clearing heat, eliminating dampness, killing parasites and detoxifying, can clear stomach and moisten intestines, and can treat eruptive abdominal pain, acute ascaris obstructive ileus and the like.
Benzopyrenes, also known as 3, 4-benzopyrenes (Benzo (a) pyrene; 3, 4-Benzy). Benzopyrene in the tea oil can be generated in the processes of frying and storing; in order to improve the oil yield, the tea seed cake is subjected to secondary oil extraction by using an extraction solvent in the production process of a refinery, so that benzopyrene residue can be caused; in addition, if the camellia seeds are placed on the asphalt horsetail to be aired, benzopyrene residues in asphalt or automobile exhaust can be adsorbed. Benzopyrene is the most commonly detected polycyclic aromatic hydrocarbon substance in food. Benzopyrene is the most definite carcinogenic substance in polycyclic aromatic hydrocarbons and belongs to common high-activity indirect carcinogens. GB 2716 and 2005 sanitary Standard for edible vegetable oil clearly stipulates that the maximum upper limit of the content of benzopyrene in the edible oil is 10 mug/kg. With the continuous improvement of health consciousness of people, food safety is concerned more and more. The research and development of a new technology and a new method for removing benzopyrene in tea oil are very important. The existing method for separating benzopyrene from tea oil comprises the following steps: activated carbon adsorption, activated clay adsorption, high temperature vacuum deodorization, etc. However, the traditional methods have low removal rate of benzopyrene, or influence the quality and natural flavor of the tea oil in the high-temperature and high-pressure process. And the benzopyrene is removed by adopting a chemical reagent method, so that the fatty acid structure of the tea oil is easily damaged, and even new residual substances harmful to human bodies can appear.
Disclosure of Invention
Aiming at the technical problems, the invention aims to provide a method for removing benzopyrene in tea oil, which can obviously improve the removal rate of benzopyrene in tea oil, does not need high-temperature environment for reaction, does not damage the fatty acid structure of tea oil and influence the quality and flavor of tea oil, does not introduce new harmful residues, and is efficient, green and environment-friendly.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for removing benzopyrene in tea oil comprises the following steps:
(1) preparing montmorillonite hydrothermal carbon composite material:
a. adding montmorillonite into hydrochloric acid according to the mass-to-volume ratio of 1g:20-40ml, stirring, performing suction filtration, washing with deionized water to neutrality, drying at the temperature of 100-;
b. adding distilled water into the acidified montmorillonite, and uniformly stirring to obtain a mixed solution 1;
c. adding glucose 2-3 times of the mass of the acidified montmorillonite into the mixed solution 1, and uniformly stirring to obtain a mixed solution 2;
d. adding 0.01-0.02mol of ammonium ferrous sulfate into the mixed solution 2, and then uniformly stirring again to obtain a mixed solution 3;
e. reacting the mixed solution 3 at 180 ℃ for 24-36h to obtain a crude product, performing suction filtration, washing the crude product to be neutral by using deionized water, washing away grease by using absolute ethyl alcohol, and drying at 100-110 ℃ for 2h to obtain the montmorillonite hydrothermal carbon composite material;
(2) adding untreated tea oil: adding 5-10g of the montmorillonite hydrothermal carbon composite material into each liter of untreated tea oil, and fully stirring and uniformly mixing to obtain a mixture;
(3) and (3) centrifugal standing: centrifuging the mixture for 5-10min, taking out and standing for 5-10 min;
(4) freezing and layering: freezing the mixture treated in the step (3) at the temperature of between-2 and-5 ℃ until the mixture is fully condensed to obtain an upper tea oil layer, a middle montmorillonite hydrothermal carbon composite material layer and a lower moisture and residue layer;
(5) separating benzopyrene: and sucking out the upper tea oil layer, and discarding the lower water and residue layer to finish the separation and removal of benzopyrene in the tea oil.
Preferably, the concentration of hydrochloric acid in the step (1) -a is 3 mol/L.
Further, the stirring time in the step (1) -a is 24-48 h.
Further, in the step (1) -a, the acidified montmorillonite is ground and then sieved by a 200-mesh sieve.
Preferably, distilled water is added into the acidified montmorillonite in the steps (1) -b according to the mass-to-volume ratio of 1g to 30-40 ml.
Further, the centrifugal rotation speed in the step (3) is 5000-.
Preferably, the freezing temperature in step (4) is-4 ℃.
Further, the freezing time in the step (4) is 25-35 min.
Compared with the prior art, the invention has the following beneficial effects:
the separation material used in the invention is the montmorillonite hydrothermal carbon composite material, which does not have qualitative change chemical reaction with the tea oil and the benzopyrene, has no influence on the quality of the tea oil, does not destroy beneficial components in the tea oil, and does not cause the loss of the tea oil. Meanwhile, new harmful residues cannot be introduced to cause secondary pollution in the tea oil, the removal efficiency of the benzopyrene is high and can reach more than 90%, and the content of the benzopyrene in the treated tea oil sample can reach below the specified range of GB 2716-2005 edible vegetable oil health Standard. The method has the advantages of simple operation, short reaction time, safety, effectiveness, economy and environmental protection.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The materials used in the following examples are all commercially available from conventional sources.
Example 1
A method for removing benzopyrene in tea oil comprises the following steps:
(1) preparing montmorillonite hydrothermal carbon composite material:
a. adding montmorillonite into 3mol/L hydrochloric acid according to the mass volume ratio of 1g:20ml, stirring for 24h, performing suction filtration, washing with deionized water to neutrality, drying at 100 ℃ for 2h to obtain acidified montmorillonite, and grinding and sieving with a 200-mesh sieve for later use;
b. adding distilled water into the acidified montmorillonite according to the mass volume ratio of 1g to 30ml, and uniformly stirring to obtain a mixed solution 1;
c. adding glucose 2 times the mass of the acidified montmorillonite into the mixed solution 1, and uniformly stirring to obtain a mixed solution 2;
d. adding 0.02mol of ammonium ferrous sulfate into the mixed solution 2, and then uniformly stirring again to obtain a mixed solution 3;
e. reacting the mixed solution 3 at 180 ℃ for 24 hours to obtain a crude product, performing suction filtration, washing the crude product to be neutral by using deionized water, washing away grease by using absolute ethyl alcohol, and drying at 100 ℃ for 2 hours to obtain the montmorillonite hydrothermal carbon composite material;
(2) adding untreated tea oil: adding 5g of the montmorillonite hydrothermal carbon composite material into each liter of untreated tea oil, and fully stirring and uniformly mixing to obtain a mixture;
(3) and (3) centrifugal standing: centrifuging the mixture at 5500r/min for 5min, taking out and standing for 10 min;
(4) freezing and layering: freezing the mixture treated in the step (3) at-2 ℃ for 35min until the mixture is fully condensed to obtain an upper tea oil layer, a middle montmorillonite hydrothermal carbon composite material layer and a lower moisture and residue layer;
(5) separating benzopyrene: and sucking out the upper tea oil layer, and discarding the lower water and residue layer to finish the separation and removal of benzopyrene in the tea oil.
Example 2
A method for removing benzopyrene in tea oil comprises the following steps:
(1) preparing montmorillonite hydrothermal carbon composite material:
a. adding montmorillonite into 3mol/L hydrochloric acid according to the mass volume ratio of 1g:30ml, stirring for 36h, performing suction filtration, washing with deionized water to neutrality, drying at 105 ℃ for 2h to obtain acidified montmorillonite, and grinding and sieving with a 200-mesh sieve for later use;
b. adding distilled water into the acidified montmorillonite according to the mass volume ratio of 1g to 35ml, and uniformly stirring to obtain a mixed solution 1;
c. adding glucose with the mass 3 times that of the acidified montmorillonite into the mixed solution 1, and uniformly stirring to obtain a mixed solution 2;
d. adding 0.02mol of ammonium ferrous sulfate into the mixed solution 2, and then uniformly stirring again to obtain a mixed solution 3;
e. reacting the mixed solution 3 at 180 ℃ for 36 hours to obtain a crude product, performing suction filtration, washing the crude product to be neutral by using deionized water, washing away grease by using absolute ethyl alcohol, and drying at 105 ℃ for 2 hours to obtain the montmorillonite hydrothermal carbon composite material;
(2) adding untreated tea oil: adding 8g of the montmorillonite hydrothermal carbon composite material into each liter of untreated tea oil, and fully stirring and uniformly mixing to obtain a mixture;
(3) and (3) centrifugal standing: centrifuging the mixture at 6000r/min for 10min, taking out and standing for 5 min;
(4) freezing and layering: freezing the mixture treated in the step (3) at-3 ℃ for 30min until the mixture is fully condensed to obtain an upper tea oil layer, a middle montmorillonite hydrothermal carbon composite material layer and a lower moisture and residue layer;
(5) separating benzopyrene: and sucking out the upper tea oil layer, and discarding the lower water and residue layer to finish the separation and removal of benzopyrene in the tea oil.
Example 3
A method for removing benzopyrene in tea oil comprises the following steps:
(1) preparing montmorillonite hydrothermal carbon composite material:
a. adding montmorillonite into 3mol/L hydrochloric acid according to the mass volume ratio of 1g:40ml, stirring for 48h, performing suction filtration, washing with deionized water to neutrality, drying at 110 ℃ for 2h to obtain acidified montmorillonite, and grinding and sieving with a 200-mesh sieve for later use;
b. adding distilled water into the acidified montmorillonite according to the mass volume ratio of 1g to 40ml, and uniformly stirring to obtain a mixed solution 1;
c. adding glucose with the mass 3 times that of the acidified montmorillonite into the mixed solution 1, and uniformly stirring to obtain a mixed solution 2;
d. adding 0.01mol of ammonium ferrous sulfate into the mixed solution 2, and then uniformly stirring again to obtain a mixed solution 3;
e. reacting the mixed solution 3 at 180 ℃ for 36 hours to obtain a crude product, performing suction filtration, washing the crude product to be neutral by using deionized water, washing away grease by using absolute ethyl alcohol, and drying at 110 ℃ for 2 hours to obtain the montmorillonite hydrothermal carbon composite material;
(2) adding untreated tea oil: adding 8g of the montmorillonite hydrothermal carbon composite material into each liter of untreated tea oil, and fully stirring and uniformly mixing to obtain a mixture;
(3) and (3) centrifugal standing: centrifuging the mixture at 5500r/min for 10min, taking out and standing for 10 min;
(4) freezing and layering: freezing the mixture treated in the step (3) at-5 ℃ for 28min until the mixture is fully condensed to obtain an upper tea oil layer, a middle montmorillonite hydrothermal carbon composite material layer and a lower moisture and residue layer;
(5) separating benzopyrene: and sucking out the upper tea oil layer, and discarding the lower water and residue layer to finish the separation and removal of benzopyrene in the tea oil.
Example 4
A method for removing benzopyrene in tea oil comprises the following steps:
(1) preparing montmorillonite hydrothermal carbon composite material:
a. adding montmorillonite into 3mol/L hydrochloric acid according to the mass volume ratio of 1g:20ml, stirring for 24h, performing suction filtration, washing with deionized water to neutrality, drying at 105 ℃ for 2h to obtain acidified montmorillonite, and grinding and sieving with a 200-mesh sieve for later use;
b. adding distilled water into the acidified montmorillonite according to the mass volume ratio of 1g to 30ml, and uniformly stirring to obtain a mixed solution 1;
c. adding glucose 2 times the mass of the acidified montmorillonite into the mixed solution 1, and uniformly stirring to obtain a mixed solution 2;
d. adding 0.01mol of ammonium ferrous sulfate into the mixed solution 2, and then uniformly stirring again to obtain a mixed solution 3;
e. reacting the mixed solution 3 at 180 ℃ for 24 hours to obtain a crude product, performing suction filtration, washing the crude product to be neutral by using deionized water, washing away grease by using absolute ethyl alcohol, and drying at 105 ℃ for 2 hours to obtain the montmorillonite hydrothermal carbon composite material;
(2) adding untreated tea oil: adding 10g of the montmorillonite hydrothermal carbon composite material into each liter of untreated tea oil, and fully stirring and uniformly mixing to obtain a mixture;
(3) and (3) centrifugal standing: centrifuging the mixture at 5000r/min for 5min, taking out and standing for 5 min;
(4) freezing and layering: freezing the mixture treated in the step (3) at-4 ℃ for 25min until the mixture is fully condensed to obtain an upper tea oil layer, a middle montmorillonite hydrothermal carbon composite material layer and a lower moisture and residue layer;
(5) separating benzopyrene: and sucking out the upper tea oil layer, and discarding the lower water and residue layer to finish the separation and removal of benzopyrene in the tea oil.
Comparative example 1 was untreated crude tea oil.
Comparative example 2 is tea oil treated by activated carbon adsorption.
Comparative example 3 is tea oil treated by high temperature vacuum deodorization.
According to the quantitative detection and analysis method of benzopyrene in national standards GB 11765-2003 oil-tea camellia seed oil and GB/T22509-2008 determination of benzopyrene of animal and vegetable oil, the benzopyrene content of the tea oil treated in examples 1-4 and comparative examples 1-3 is subjected to comparison quantitative analysis by a benzopyrene ether solution (standard sample), a 5-point correction curve is drawn by using a standard curve method according to the chromatographic conditions listed in GB/T22509-2008, and the benzopyrene value is calculated, and the results are shown in the following table.
TABLE 1 Effect of different treatments on the content of benzopyrene in tea oil
As can be seen from the data in Table 1, the content of benzopyrene in the crude tea oil which is not treated in comparative example 1 reaches 16.2983 mug/mL, which is far higher than the highest upper limit of the content of benzopyrene in the edible oil specified in GB 2716-2005 edible vegetable oil sanitation Standard. The content of benzopyrene in the tea oil treated by the activated carbon adsorption method of the comparative example 2 is reduced to be below the standard, but the removal rate is still low and is only 59.36%. Comparative example 3 the removal rate of benzopyrene in the tea oil treated by the high temperature vacuum deodorization method is improved, but the fatty acid structure part of the tea oil is damaged at high temperature, and the natural flavor of the tea oil such as transparency, color, smell and taste is also influenced by different degrees.
The removal rate of benzopyrene in the embodiments 1-4 adopting the removal method provided by the application is more than 90%, wherein the best effect is embodiment 4, 94.43% is achieved, and the separation effect is obvious. Meanwhile, the method does not need high temperature, basically does not influence the quality index of the tea oil, and has the advantages of simple operation, short reaction time, safety, effectiveness, economy and environmental protection.
Claims (8)
1. A method for removing benzopyrene in tea oil is characterized by comprising the following steps:
(1) preparing montmorillonite hydrothermal carbon composite material:
a. adding montmorillonite into hydrochloric acid according to the mass-to-volume ratio of 1g:20-40ml, stirring, performing suction filtration, washing with deionized water to neutrality, drying at the temperature of 100-;
b. adding distilled water into the acidified montmorillonite, and uniformly stirring to obtain a mixed solution 1;
c. adding glucose 2-3 times of the mass of the acidified montmorillonite into the mixed solution 1, and uniformly stirring to obtain a mixed solution 2;
d. adding 0.01-0.02mol of ammonium ferrous sulfate into the mixed solution 2, and then uniformly stirring again to obtain a mixed solution 3;
e. reacting the mixed solution 3 at 180 ℃ for 24-36h to obtain a crude product, performing suction filtration, washing the crude product to be neutral by using deionized water, washing away grease by using absolute ethyl alcohol, and drying at 100-110 ℃ for 2h to obtain the montmorillonite hydrothermal carbon composite material;
(2) adding untreated tea oil: adding 5-10g of the montmorillonite hydrothermal carbon composite material into each liter of untreated tea oil, and fully stirring and uniformly mixing to obtain a mixture;
(3) and (3) centrifugal standing: centrifuging the mixture for 5-10min, taking out and standing for 5-10 min;
(4) freezing and layering: freezing the mixture treated in the step (3) at the temperature of between-2 and-5 ℃ until the mixture is fully condensed to obtain an upper tea oil layer, a middle montmorillonite hydrothermal carbon composite material layer and a lower moisture and residue layer;
(5) separating benzopyrene: and sucking out the upper tea oil layer, and discarding the lower water and residue layer to finish the separation and removal of benzopyrene in the tea oil.
2. The method for removing benzopyrene in tea oil according to claim 1, wherein the concentration of hydrochloric acid in the step (1) -a is 3 mol/L.
3. The method for removing benzopyrene in tea oil according to claim 1, wherein the stirring time in the step (1) -a is 24-48 h.
4. The method for removing benzopyrene in tea oil according to claim 1, wherein the acidified montmorillonite in step (1) -a is ground and then sieved by a 200-mesh sieve.
5. The method for removing benzopyrene in tea oil according to claim 1, wherein distilled water is added to the acidified montmorillonite in the step (1) -b according to the mass-to-volume ratio of 1g to 30-40 ml.
6. The method for removing benzopyrene in tea oil as claimed in claim 1, wherein the centrifugation rotation speed in step (3) is 5000-.
7. The method for removing benzopyrene in tea oil according to claim 1, wherein the freezing temperature in the step (4) is-4 ℃.
8. The method for removing benzopyrene in tea oil according to claim 1 or 7, wherein the freezing time in the step (4) is 25-35 min.
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| CN115475400A (en) * | 2022-09-30 | 2022-12-16 | 湘南学院 | Method for removing polycyclic aromatic hydrocarbon in tea oil by molecular distillation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115475400A (en) * | 2022-09-30 | 2022-12-16 | 湘南学院 | Method for removing polycyclic aromatic hydrocarbon in tea oil by molecular distillation |
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Application publication date: 20200207 |