CN109603201B - Method for removing benzoic acid from Capsici fructus extract - Google Patents
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Abstract
A method for removing benzoic acid from a pepper extract comprises the following steps: (1) adding an alcohol aqueous solution into the pepper extract, uniformly stirring at 41-50 ℃, standing for layering, obtaining a solution II on the upper layer, and obtaining a solution I on the lower layer; (2) removing the organic solvent from the solution I to obtain a pepper extract I qualified in benzoic acid; (3) adding a low-concentration alcohol water solution into the solution II to dilute until the alcohol content is 80-85%, adjusting the pH value to be less than or equal to 2, heating, passing through macroporous adsorption resin, and collecting column-passing liquid; (4) and adding pure water into the column passing liquid until the alcohol content is less than or equal to 10%, adjusting the pH value to 7-10, stirring and uniformly mixing, centrifuging to remove a water layer, and removing the organic solvent to obtain the pepper extract II with qualified benzoic acid. The method can maximize the removal rate of benzoic acid in the pepper extract by an organic solvent method and a macroporous adsorption resin method, has simple process and low cost, and is suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of removing noxious substances in natural extracts, and particularly relates to a method for removing benzoic acid in a pepper extract.
Background
Benzoic acid is widely used as a food preservative, but the excessive long-term consumption of benzoic acid can damage the functions of liver and kidney of human bodies, so that countries in the world have strict limits on the content of benzoic acid in food and food additives, national standards of China also clearly stipulate the maximum using amount (200-1500 mg/kg) of benzoic acid in 22 types of food, and the addition of benzoic acid as the preservative is not allowed in the foods except the 22 types of food.
However, there are many reports in the literature that benzoic acid is a secondary metabolite of plants and naturally exists in various plants such as pepper. The capsicum extract is extracted from capsicum, and in the production processes of extraction, concentration and the like, benzoic acid is transferred and enriched into the capsicum extract, so that the large-scale and wide-scale use of the capsicum extract has potential food safety hazards, and the healthy development of the capsicum extract industry is influenced. Therefore, it is necessary to develop a method for removing benzoic acid from a capsicum extract.
At present, the literature reports about removing benzoic acid mainly aim at industrial wastewater, the removal technology mainly comprises biological carbon, flocculation of anionic surfactant and aluminum salt adsorption micelle, macroporous adsorption resin, modified bentonite, enzyme preparation and the like, and no literature reports about a method for removing benzoic acid in a pepper extract. The pepper extract is a mixture of pepper pigment, capsaicin and pepper oil and fat, and the stability of target components is poor, so that a method for removing benzoic acid, which can be industrially produced and does not influence the yield of the target components, is sought, and the technical problem to be solved is needed at present.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for removing benzoic acid in a pepper extract, and the benzoic acid in the pepper extract is removed to the maximum extent under the condition of not influencing the yield of target components.
In order to solve the technical problems, the invention adopts the technical scheme that: a method for removing benzoic acid from a pepper extract comprises the following steps:
(1) adding an alcohol aqueous solution into the pepper extract, uniformly stirring at 41-50 ℃, standing for layering, obtaining a solution II on the upper layer, and obtaining a solution I on the lower layer;
(2) removing the organic solvent from the solution I through a deodorizing pot to obtain a pepper extract I qualified in benzoic acid;
(3) adding a low-concentration alcohol water solution into the solution II to dilute until the alcohol content is 80-85%, adjusting the pH value to be less than or equal to 2, heating to 41-50 ℃, passing through macroporous adsorption resin, and collecting column-passing liquid;
(4) and adding pure water into the column passing liquid until the alcohol content is less than or equal to 10%, adding alkali liquor to adjust the pH value to 7-10, stirring and mixing uniformly, centrifuging to stratify, removing a water layer, and removing the organic solvent through a deodorizing pot to obtain the pepper extract II with qualified benzoic acid.
The alcohol-water solution in the step (1) is a methanol water solution or an ethanol water solution with a volume ratio of 91: 9-95: 5, and the mass-volume ratio of the pepper extract to the alcohol-water solution is 1: 3-4;
the low-concentration alcohol water solution in the step (3) is a methanol water solution or an ethanol water solution with the volume ratio of 5: 95-20: 80; the macroporous adsorption resin is NKA-II, SD300 or XDA-1, and the adsorption flow rate is 1-3 BV/h; the solution used for adjusting the pH value is a citric acid aqueous solution with the mass fraction of 1-5 per mill.
The alkali liquor in the step (4) is a sodium hydroxide solution or a sodium bicarbonate solution with the mass fraction of 1-3 per mill; the centrifugal equipment is a horizontal screw centrifuge, and the separation factor is 6000.
The temperature for removing the organic solvent in the step (2) and the step (4) is 45-50 ℃, and the vacuum degree is more than or equal to 0.085 MPa; the stirring speed of the deodorizing pot is 60-80 r/min.
Adopt above-mentioned technical scheme's beneficial effect to lie in: (1) separating the precipitate of Capsici fructus extract with ethanol water solution to obtain Capsici fructus extract I with qualified benzoic acid, and separating target components in Capsici fructus extract; (2) the removal rate of benzoic acid in the pepper extract II is maximized through the combined action of a macroporous adsorption resin method and an organic solvent method; (3) pure water is added into the column passing liquid to separate out the pepper extract, thereby not only ensuring the yield of the pepper extract, but also removing water-soluble impurities in the pepper extract and improving the product quality; (4) after the macroporous adsorption resin is saturated in adsorbing benzoic acid, the benzoic acid can be repeatedly used after being eluted and regenerated by a sodium hydroxide solution, so that the removal cost is reduced; (5) the invention has simple process and low cost, and is suitable for industrial production.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
(1) Adding 60L ethanol water solution with volume ratio of 91:9 into 20kg of pepper extract, stirring and mixing uniformly at 50 ℃, standing for precipitation and layering to obtain solution II on the upper layer and solution I on the lower layer;
(2) removing organic solvent from the obtained solution I at 45 deg.C and vacuum degree of 0.085MPa in a deodorizing pot at rotation speed of 70r/min to obtain Capsici fructus extract I;
(3) adding the obtained solution II into the solution in a volume ratio of 5: diluting 95 ethanol water solution to 80% ethanol content, adding 1 ‰ citric acid water solution by mass fraction to adjust pH to 2 or less, heating to 45 deg.C, passing through NKA-II macroporous adsorbent resin at adsorption flow rate of 1BV/h, and collecting column-passing solution;
(4) adding pure water into the obtained column passing liquid until the ethanol content is 8%, adding 1 per mill of sodium hydroxide solution by mass percent to adjust the pH value to 7.0, stirring and mixing uniformly, centrifuging and layering by a horizontal screw centrifuge with a separation factor of 6000, removing a water layer, and removing an organic solvent by a deodorizing pot with a rotating speed of 70r/min under the condition of a vacuum degree of 0.085MPa at 45 ℃ to obtain the chilli extract II with qualified benzoic acid.
According to detection, the content of benzoic acid in the raw material pepper extract is 24.2mg/kg, benzoic acid is not detected in the pepper extract I and the pepper extract II after benzoic acid is removed, and the detection limit of the method is 2 mg/kg.
Example 2
(1) Adding 70L methanol water solution with volume ratio of 95:5 into 20kg of pepper extract, stirring and mixing uniformly at 45 ℃, standing and precipitating for layering, wherein the upper layer obtains a solution II, and the lower layer obtains a solution I;
(2) removing organic solvent from the obtained solution I at 47 deg.C and vacuum degree of 0.090MPa in a deodorizing pot at rotation speed of 80r/min to obtain Capsici fructus extract I;
(3) adding the obtained solution II into the reactor in a volume ratio of 10: diluting 90 methanol aqueous solution until the methanol content is 82%, adding 2 per mill citric acid aqueous solution by mass to adjust the pH to be less than or equal to 2, heating to 50 ℃, passing through SD300 macroporous adsorption resin at the adsorption flow rate of 2BV/h, and collecting column passing liquid;
(4) and adding pure water into the obtained column passing liquid until the content of methanol is 7%, adding 3 per mill of sodium bicarbonate solution by mass percent, adjusting the pH value to 7.5, stirring and uniformly mixing, centrifuging and layering by a horizontal screw centrifuge with a separation factor of 6000, removing a water layer, and removing the organic solvent by a deodorizing pot with a rotating speed of 80r/min under the condition of a vacuum degree of 0.090MPa at 47 ℃ to obtain the pepper extract II with qualified benzoic acid.
Detection shows that the content of benzoic acid in the raw material pepper extract is 23.5mg/kg, no benzoic acid is detected in the pepper extract I and the pepper extract II after benzoic acid is removed, and the detection limit of the method is 2 mg/kg.
Example 3
(1) Adding 80L ethanol water solution with volume ratio of 93:7 into 20kg Capsici fructus extract, stirring at 41 deg.C, standing for precipitation, layering to obtain upper layer solution II and lower layer solution I;
(2) removing organic solvent from the obtained solution I at 50 deg.C and vacuum degree of 0.095MPa in a deodorizing pot at rotation speed of 60r/min to obtain Capsici fructus extract I;
(3) adding an ethanol water solution with the volume ratio of 20:80 into the obtained solution II to dilute until the ethanol content is 85%, adding a citric acid water solution with the mass fraction of 5 per mill to adjust the pH value to be less than or equal to 2, heating to 48 ℃, passing through XDA-1 macroporous adsorption resin at the adsorption flow rate of 3BV/h, and collecting the column passing liquid;
(4) and adding pure water into the obtained column passing liquid until the ethanol content is 9%, adding 2 per mill of sodium bicarbonate solution by mass percent, adjusting the pH value to 8.0, stirring and uniformly mixing, centrifuging and layering by a horizontal screw centrifuge with a separation factor of 6000, removing a water layer, and removing the organic solvent by a deodorizing pot of 60r/min under the condition of a vacuum degree of 0.095MPa at 50 ℃ to obtain the pepper extract II with qualified benzoic acid.
According to detection, the content of benzoic acid in the raw material pepper extract is 25.0mg/kg, benzoic acid is not detected in the pepper extract I and the pepper extract II after benzoic acid is removed, and the detection limit of the method is 2 mg/kg.
Example 4
(1) Adding 400L of methanol aqueous solution with volume ratio of 92:8 into 100kg of pepper extract, stirring and mixing uniformly at 44 ℃, standing for precipitation and layering, wherein the upper layer is solution II and the lower layer is solution I;
(2) removing organic solvent from the obtained solution I at 47 deg.C and vacuum degree of 0.090MPa in a deodorizing pot at 65r/min to obtain Capsici fructus extract I;
(3) adding the obtained solution II into the solution in a volume ratio of 8: diluting the 92 methanol aqueous solution to the content of 82% methanol, adding 3 per mill citric acid aqueous solution by mass to adjust pH to 2 or less, heating to 42 deg.C, passing through XDA-1 porous adsorption resin at adsorption flow rate of 1.5BV/h, and collecting the column-passing solution;
(4) and adding pure water into the obtained column passing liquid until the content of methanol is 10%, adding sodium bicarbonate solution with the mass fraction of 1.5 per mill to adjust the pH value to 8.5, stirring and uniformly mixing, centrifuging and layering by a horizontal screw centrifuge with the separation factor of 6000, removing a water layer, and removing the organic solvent by a deodorizing pot with the rotating speed of 65r/min under the condition of the vacuum degree of 0.085MPa at 50 ℃ to obtain the chilli extract II with qualified benzoic acid.
According to detection, the content of benzoic acid in the raw material pepper extract is 25.8mg/kg, benzoic acid is not detected in the pepper extract I and the pepper extract II after benzoic acid is removed, and the detection limit of the method is 2 mg/kg.
Example 5
(1) Adding 380L methanol aqueous solution with the volume ratio of 93:7 into 100kg of pepper extract, stirring and uniformly mixing at 50 ℃, standing, precipitating and layering to obtain a solution II on the upper layer and a solution I on the lower layer;
(2) removing organic solvent from the obtained solution I at 46 deg.C and vacuum degree of 0.095MPa in a deodorizing pot at rotation speed of 75r/min to obtain Capsici fructus extract I;
(3) adding the obtained solution II into the solution in a volume ratio of 17: diluting the 83 methanol aqueous solution to 83% methanol content, adding 2 ‰ citric acid aqueous solution by mass to adjust pH to 2 or less, heating to 45 deg.C, passing through SD300 macroporous adsorbent resin at adsorption flow rate of 1BV/h, and collecting the column-passing solution;
(4) and adding pure water into the obtained column passing liquid until the content of methanol is 3%, adding 2 per mill of sodium hydroxide solution by mass percent, adjusting the pH value to 9.0, stirring and uniformly mixing, centrifuging and layering by a horizontal screw centrifuge with a separation factor of 6000, removing a water layer, and removing the organic solvent by a deodorizing pot with a rotating speed of 80r/min under the condition of a vacuum degree of 0.095MPa at 46 ℃ to obtain the chilli extract II with qualified benzoic acid.
Detection shows that the content of benzoic acid in the raw material pepper extract is 22.6mg/kg, no benzoic acid is detected in the pepper extract I and the pepper extract II after benzoic acid is removed, and the detection limit of the method is 2 mg/kg.
Example 6
(1) Adding 160L ethanol water solution with volume ratio of 95:5 into 50kg of pepper extract, stirring and mixing uniformly at 48 ℃, standing for precipitation and layering, wherein the upper layer is solution II, and the lower layer is solution I;
(2) removing organic solvent from the obtained solution I at 47 deg.C and vacuum degree of 0.10MPa in a deodorizing pot at rotation speed of 78r/min to obtain Capsici fructus extract I;
(3) adding the obtained solution II into the solution in a volume ratio of 20: diluting 80 ethanol water solution until the ethanol content is 85%, adding 1 per mill citric acid water solution by mass fraction to adjust pH to 2 or less, heating to 47 deg.C, passing through SD300 macroporous adsorbent resin at adsorption flow rate of 2.5BV/h, and collecting column-passing solution;
(4) and adding pure water into the obtained column passing liquid until the ethanol content is 2%, then adding 1 per mill of sodium bicarbonate solution by mass fraction to adjust the pH value to 9.5, stirring and uniformly mixing, centrifuging and layering by a horizontal screw centrifuge with a separation factor of 6000, removing a water layer, and removing the organic solvent by a deodorizing pot with a rotating speed of 62r/min under the condition of a vacuum degree of 0.090MPa at 48 ℃ to obtain the pepper extract II with qualified benzoic acid.
Detection shows that the content of benzoic acid in the raw material pepper extract is 23.3mg/kg, no benzoic acid is detected in the pepper extract I and the pepper extract II after benzoic acid is removed, and the detection limit of the method is 2 mg/kg.
Example 7
(1) Adding 180L ethanol water solution with volume ratio of 94:6 into 50kg of Capsici fructus extract, stirring and mixing at 46 deg.C, standing for precipitation and layering to obtain solution II on the upper layer and solution I on the lower layer;
(2) removing organic solvent from the obtained solution I at 50 deg.C and vacuum degree of 0.090MPa in a deodorizing pot at rotation speed of 62r/min to obtain Capsici fructus extract I;
(3) adding the obtained solution II into the reactor in a volume ratio of 12: 88, diluting the ethanol aqueous solution until the methanol content is 83%, adding 4 per mill citric acid aqueous solution by mass percent to adjust the pH value to be less than or equal to 2, heating to 41 ℃, passing through XDA-1 macroporous adsorption resin at the adsorption flow rate of 1BV/h, and collecting the column passing liquid;
(4) and adding pure water into the obtained column passing liquid until the content of methanol is 10%, adding 3 per mill of sodium hydroxide solution by mass percent, adjusting the pH value to 10.0, stirring and uniformly mixing, centrifuging and layering by a horizontal screw centrifuge with a separation factor of 6000, removing a water layer, and removing the organic solvent by a deodorizing pot at the rotating speed of 77r/min under the condition of the vacuum degree of 0.095MPa at 45 ℃ to obtain the chilli extract II with qualified benzoic acid.
According to detection, the content of benzoic acid in the raw material pepper extract is 25.4mg/kg, benzoic acid is not detected in the pepper extract I and the pepper extract II after benzoic acid is removed, and the detection limit of the method is 2 mg/kg.
Example 8
(1) Adding 75L methanol water solution with volume ratio of 91:9 into 20kg Capsici fructus extract, stirring at 45 deg.C, standing for precipitation and layering to obtain solution II on the upper layer and solution I on the lower layer;
(2) removing organic solvent from the obtained solution I at 48 deg.C and vacuum degree of 0.085MPa in a deodorizing pot at rotation speed of 60r/min to obtain Capsici fructus extract I;
(3) adding the obtained solution II into the solution in a volume ratio of 15: 85, diluting the methanol aqueous solution until the methanol content is 84%, adding 3 per mill of citric acid aqueous solution by mass fraction to adjust the pH value to be less than or equal to 2, heating to 43 ℃, passing through NKA-II macroporous adsorption resin at the adsorption flow rate of 2.5BV/h, and collecting the column passing liquid;
(4) and adding pure water into the obtained column passing liquid until the content of methanol is 2.5%, adding 5 per mill of sodium bicarbonate solution by mass percent, adjusting the pH value to 8.0, stirring and uniformly mixing, centrifuging and layering by a horizontal screw centrifuge with a separation factor of 6000, removing a water layer, and removing an organic solvent by a deodorizing pot with a rotating speed of 70r/min under the condition of a vacuum degree of 0.10MPa at 46 ℃ to obtain the chilli extract II with qualified benzoic acid.
According to detection, the content of benzoic acid in the raw material pepper extract is 21.2mg/kg, benzoic acid is not detected in the pepper extract I and the pepper extract II after benzoic acid is removed, and the detection limit of the method is 2 mg/kg.
Example 9
(1) Adding 330L methanol water solution with volume ratio of 94:6 into 100kg Capsici fructus extract, stirring at 42 deg.C, standing for precipitation, layering to obtain solution II on the upper layer and solution I on the lower layer;
(2) removing organic solvent from the obtained solution I at 48 deg.C and vacuum degree of 0.085MPa in a deodorizing pot at rotation speed of 66r/min to obtain Capsici fructus extract I;
(3) adding the obtained solution II into the solution in a volume ratio of 7: 93 diluting the methanol aqueous solution until the methanol content is 82%, adding 5 per mill of citric acid aqueous solution by mass percent to adjust the pH value to be less than or equal to 2, heating to 50 ℃, passing through NKA-II macroporous adsorption resin at the adsorption flow rate of 2BV/h, and collecting the column passing liquid;
(4) and adding pure water into the obtained column passing liquid until the content of methanol is 6%, adding a sodium hydroxide solution with the mass fraction of 2.5 per mill to adjust the pH value to 9.0, stirring and uniformly mixing, centrifuging and layering by a horizontal screw centrifuge with the separation factor of 6000, removing a water layer, and removing the organic solvent by a deodorizing pot with the rotating speed of 80r/min under the condition of the vacuum degree of 0.10MPa at 47 ℃ to obtain the chilli extract II with qualified benzoic acid.
According to detection, the content of benzoic acid in the raw material pepper extract is 24.9mg/kg, benzoic acid is not detected in the pepper extract I and the pepper extract II after benzoic acid is removed, and the detection limit of the method is 2 mg/kg.
Claims (4)
1. The method for removing benzoic acid in the pepper extract is characterized by comprising the following steps of:
(1) adding an alcohol aqueous solution into the pepper extract, uniformly stirring at 41-50 ℃, standing for layering, obtaining a solution II on the upper layer, and obtaining a solution I on the lower layer;
(2) removing the organic solvent from the solution I through a deodorizing pot to obtain a pepper extract I qualified in benzoic acid;
(3) adding a low-concentration alcohol water solution into the solution II to dilute until the alcohol content is 80-85%, adjusting the pH value to be less than or equal to 2, heating to 41-50 ℃, passing through macroporous adsorption resin, and collecting column-passing liquid;
(4) adding pure water into the column passing liquid until the alcohol content is less than or equal to 10%, adding alkali liquor to adjust the pH value to 7-10, stirring and mixing uniformly, centrifuging and layering, removing a water layer, and removing an organic solvent through a deodorizing pot to obtain a pepper extract II with qualified benzoic acid;
the alcohol-water solution in the step (1) is a methanol water solution or an ethanol water solution with a volume ratio of 91: 9-95: 5, and the mass-volume ratio of the pepper extract to the alcohol-water solution is 1: 3-4;
the low-concentration alcohol water solution in the step (3) is a methanol water solution or an ethanol water solution with the volume ratio of 5: 95-20: 80; the macroporous adsorption resin is NKA-II, SD300 or XDA-1, and the adsorption flow rate is 1-3 BV/h;
the alkali liquor in the step (4) is a sodium hydroxide solution or a sodium bicarbonate solution with the mass fraction of 1-3 per mill;
the temperature for removing the organic solvent in the step (2) and the step (4) is 45-50 ℃, and the vacuum degree is more than or equal to 0.085 MPa.
2. The method for removing benzoic acid from a pepper extract as claimed in claim 1, wherein the stirring speed of the deodorizing pot in the steps (2) and (4) is 60-80 r/min.
3. The method for removing benzoic acid from a pepper extract as claimed in claim 1, wherein the step (3) uses an aqueous solution of citric acid with a mass fraction of 1-5% o to adjust the pH value.
4. The method for removing benzoic acid from a capsicum extract according to claim 1, 2 or 3, wherein the centrifugation device of the step (4) is a horizontal screw centrifuge with a separation factor of 6000.
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