CN102433072B - Method for removing rhodamine B in capsicum oleoresin - Google Patents
Method for removing rhodamine B in capsicum oleoresin Download PDFInfo
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- CN102433072B CN102433072B CN2011102837619A CN201110283761A CN102433072B CN 102433072 B CN102433072 B CN 102433072B CN 2011102837619 A CN2011102837619 A CN 2011102837619A CN 201110283761 A CN201110283761 A CN 201110283761A CN 102433072 B CN102433072 B CN 102433072B
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Abstract
The invention discloses a method for removing rhodamine B in capsicum oleoresin, comprising the following processing steps of: 1, dissolving the capsicum oleoresin containing the rhodamine B into an esters solvent or an alkanes solvent and stirring uniformly to obtain resin solution; 2, adding alcohol-water solution to the resin solution and stirring to mix uniformly to obtain mixed solution, in which a molecular weight of the alcohol in the alcohol-water solution is lower than that of the esters solvent or the alkanes solvent; 3, standing the mixed solution or centrifugalizing to layer to separate out an alcohol layer, thus obtaining an esters solvent layer or an alkanes solvent layer; 4, adding salt solution to the esters solvent layer or the alkanes solvent layer and stirring uniformly; then, standing or centrifugalizing to layer to separate out a saltwater layer on the lower layer; and 5, concentrating the esters solvent layer or the alkanes solvent layer after separating the saltwater layer, and removing solvent residue to obtain the capsicum oleoresin without the rhodamine B. The method has simple process and convenience in operation, can obtain the capsicum oleoresin without the rhodamine B and can realize industrialization production.
Description
Technical field
The present invention relates to a kind of method of purification of oleoresin capsicum, the removal method of rhodamine B in especially a kind of oleoresin capsicum.
Background technology
Capsicum is as most important sharp flavor seasoning good merchantable brand, and is indispensable in food-processing.Oleoresin capsicum is a kind of oily liquids that extracts from capsicum, the strong sharp flavor that has kept capsicum, and have pungency component quantification, stdn, easy to use, low cost and other advantages, replace in a large number capsicum to be widely used in the industries such as food, seasonings.
Rhodamine B (Rhodamine B) claim again rose red b, or basic rhodamine, and it is red to be commonly called as pollen, is a kind of bright pinkish synthetic dyestuff that has.Find that through pharmacological testing rhodamine B can cause subcutis raw meat knurl, under a cloud is carcinogenic substance, and shows that without any rules it is safe that rhodamine B is used in the food at present.Chongqing and Hunan Entry-Exit Inspection and Quarantine Bureau unite formulation and standard " detection method of rhodamine B in the SNT 2430-2010 import and export food ", use the LC-MS instrument to detect, become the authoritative standard of the supervision of rhodamine B in the product and quality control, it detects and is limited to 5ppb.
Find by long-term monographic study, in the oleoresin capsicum product that enterprise produces both at home and abroad, some can detect the rhodamine B of trace or trace, wherein the external product average content is higher than domestic, although mechanism is still not clear, and with regard to content, also be not enough to human body is worked the mischief, but its character and making a very bad impression, especially contain the harm composition in the homemade goods, if can not effectively remove, improve security, on the one hand under the severe situation of food safety, can cause human consumer's fear at heart, will produce directly the international image of industry healthy development and viewpoint of Chinese food safety on the other hand and impact.
The oleoresin capsicum of China has occupied about 40% of international market share, but in view of numerous food product additive food safety of enterprises is realized thin, detection level is limited, the factors such as the technique research and development ability is weak, rhodamine B in the oleoresin capsicum product not yet causes enough attention, the enterprise that has even the safety index of its product known nothing hides some dangers for to industry development.Up to now, there is no the open report of removing trace in the oleoresin capsicum or trace rhodamine B, develop a kind of like this technique, comply with on the one hand the food safety development situation, on the other hand by improving Product Safety, can strengthen the synthesized competitiveness of product, and to improving competitiveness in the international market, have very large realistic meaning.
Summary of the invention
The technical problem to be solved in the present invention provides the removal method of rhodamine B in a kind of oleoresin capsicum, with the rhodamine B in the effective removal oleoresin capsicum.
For solving the problems of the technologies described above, the technical solution used in the present invention is: the processing step of the method is:
The oleoresin capsicum that (1) will contain rhodamine B is dissolved in esters solvent or the alkane solvents, stirs, and obtains resin solution;
(2) add alcohol solution in resin solution, stirring mixes it, obtains mixed solution; The molecular weight of alcohol is lower than the molecular weight of esters solvent or alkane solvents in the described alcohol solution;
(3) the alcohol layer is told in mixed solution standing demix or centrifugal layering; Obtain esters solvent layer or alkane solvents layer;
(4) esters solvent layer or alkane solvents layer add salt solution, stir; Then the brine layer of lower floor is told in standing demix or centrifugal layering;
(5) divide the esters solvent layer behind the water layer that desalts or the alkane solvents layer is concentrated and desolvation is residual, can obtain removing the oleoresin capsicum of rhodamine B.
Esters solvent in the step of the present invention (1) is ethyl acetate or propyl acetate; Described alkane solvents is normal hexane or hexanaphthene; Every kilogram of oleoresin capsicum is dissolved in 8～10L esters solvent or the alkane solvents.
The volume fraction of alcohol solution is 30%～50% in the step of the present invention (2), and the alcohol in the described alcohol solution is ethanol or methyl alcohol; Every kilogram of oleoresin capsicum adds 2～4L alcohol solution.
Standing demix in the step of the present invention (3) is that mixed solution leaves standstill layering after 0.5～2 hour.
The massfraction of salt solution is 3 ‰ in the step of the present invention (4), and every kilogram of oleoresin capsicum adds 3～5L salt solution; Standing demix in the described step (4) is for leaving standstill layering after 0.5～2 hour.
Step of the present invention (3) obtains the esters solvent layer or the alkane solvents layer is washed 4～5 times with alcohol solution according to step (2)-(3) again.
The solubleness of rhodamine B in alcoholic solution is larger, oleoresin capsicum is dispersed in first in ester class or the alkane solvents, with the alcoholic solvent of certain number of degrees rhodamine B is competed out from ester class or alkane solvents layer again, most peppery degree is stayed in ester class or the alkane solvents.With salt solution esters solvent layer or alkane solvents layer are cleaned, on the one hand a part of water-soluble impurity in the oleoresin capsicum is washed out, also be wrapped with simultaneously the rhodamine B of trace in the impurity.The oleoresin capsicum that obtains does not contain rhodamine B.
The beneficial effect that adopts technique scheme to produce is: technique of the present invention is simple, easy to operate, can not contained the oleoresin capsicum of the high security of rhodamine B, and can realize suitability for industrialized production.
Embodiment
The present invention is further detailed explanation below in conjunction with specific embodiment.
Embodiment 1: the removal method of rhodamine B adopts following processing step in this oleoresin capsicum.
(1) be 25ppb with rhodamine B content, peppery degree is that 10.1% oleoresin capsicum 50.0kg is dissolved in the 500L ethyl acetate, stirs, and obtains resin solution;
(2) add the 40%(volume fraction in the above-mentioned resin solution) aqueous ethanolic solution 150L, stir it mixed, obtain mixed solution;
(3) standing demix: above-mentioned mixed solution was left standstill 0.5 hour, and mixed solution is layered as alcohol layer and ethyl acetate layer, then the alcohol layer is told;
(4) ethyl acetate layer is washed 4 times by step (2)-(3);
(5) will washing ethyl acetate layer after 4 times, to add massfraction be 3 ‰ salt solution 200L, stirs; Left standstill 1 hour, and be layered as ethyl acetate layer and brine layer; Brine layer is told;
(6) concentrated, desolvation is residual: will the ethyl acetate layer in (5) step concentrated desolvation be residual afterwards, obtains oleoresin capsicum 40.3kg, peppery degree 11.52%; According to " detection method of rhodamine B in the SNT 2430-2010 import and export food ", use the rhodamine B in the LC-MS instrument testing product, do not detect.
Embodiment 2: the removal method of rhodamine B adopts following processing step in this oleoresin capsicum.
(1) be 38ppb with rhodamine B content, peppery degree is that 16.2% oleoresin capsicum 50.0kg is dissolved in the 400L propyl acetate, stirs, and obtains resin solution;
(2) add the 30%(volume fraction in the above-mentioned resin solution) methanol aqueous solution 100L, stir it mixed, obtain mixed solution;
(3) centrifugal layering: use separating machine to be separated into alcohol layer and propyl acetate layer above-mentioned mixed solution, then the alcohol layer is told;
(4) the propyl acetate layer is washed 4 times by step (2)-(3);
(5) will washing 4 times propyl acetate layer, to add massfraction be 3 ‰ salt solution 150L, stirs; Left standstill 0.5 hour, and be layered as propyl acetate layer and brine layer; Brine layer is told;
(6) concentrated, desolvation is residual: will the propyl acetate layer in (5) step concentrated desolvation be residual afterwards, obtains oleoresin capsicum 41.1kg, peppery degree 17.3%; According to " detection method of rhodamine B in the SNT 2430-2010 import and export food ", use the rhodamine B in the LC-MS instrument testing product, do not detect.
Embodiment 3: the removal method of rhodamine B adopts following processing step in this oleoresin capsicum.
(1) be 30ppb with rhodamine B content, peppery degree is that 13.2% oleoresin capsicum 50.0kg is dissolved in the 400L normal hexane, stirs, and obtains resin solution;
(2) add the 50%(volume fraction in the above-mentioned resin solution) methanol aqueous solution 200L, stir it mixed, obtain mixed solution;
(3) centrifugal layering: use separating machine to be separated into alcohol layer and normal hexane layer above-mentioned mixed solution, then the alcohol layer is told;
(4) the normal hexane layer is washed 5 times by step (2)-(3);
(5) will washing 5 times normal hexane layer, to add massfraction be 3 ‰ salt solution 250L, stirs; Left standstill 2 hours, and be layered as normal hexane layer and brine layer; Brine layer is told;
(6) concentrated, desolvation is residual: will the normal hexane layer in (5) step concentrated desolvation be residual afterwards, obtains oleoresin capsicum 42.3kg, peppery degree 14.8%; According to " detection method of rhodamine B in the SNT 2430-2010 import and export food ", use the rhodamine B in the LC-MS instrument testing product, do not detect.
Embodiment 4: the removal method of rhodamine B adopts following processing step in this oleoresin capsicum.
(1) be 30ppb with rhodamine B content, peppery degree is that 15.4% oleoresin capsicum 50.0kg is dissolved in the 450L hexanaphthene, stirs, and obtains resin solution;
(2) add the 45%(volume fraction in the above-mentioned resin solution) aqueous ethanolic solution 150L, stir it mixed, obtain mixed solution;
(3) standing demix: above-mentioned mixed solution was left standstill 2 hours, and mixed solution is layered as alcohol layer and hexanaphthene layer, then the alcohol layer is told;
(4) the hexanaphthene layer is washed 5 times by step (2)-(3);
(5) will washing 5 times hexanaphthene layer, to add massfraction be 3 ‰ salt solution 200L, stirs; Left standstill 1.5 hours, and be layered as hexanaphthene layer and brine layer; Brine layer is told;
(6) concentrated, desolvation is residual: will the hexanaphthene layer in (5) step concentrated desolvation be residual afterwards, obtains oleoresin capsicum 41.8kg, peppery degree 16.9%; According to " detection method of rhodamine B in the SNT 2430-2010 import and export food ", use the rhodamine B in the LC-MS instrument testing product, do not detect.
Claims (6)
1. the removal method of rhodamine B in the oleoresin capsicum is characterized in that the processing step of the method is:
The oleoresin capsicum that (1) will contain rhodamine B is dissolved in esters solvent or the alkane solvents, stirs, and obtains resin solution; Described esters solvent is ethyl acetate or propyl acetate; Described alkane solvents is normal hexane or hexanaphthene;
(2) add alcohol solution in resin solution, stirring mixes it, obtains mixed solution; Alcohol in the described alcohol solution is ethanol or methyl alcohol, and the molecular weight of alcohol is lower than the molecular weight of esters solvent or alkane solvents; The volume fraction of described alcohol solution is 30%～50%;
(3) the alcohol layer is told in mixed solution standing demix or centrifugal layering; Obtain esters solvent layer or alkane solvents layer;
(4) esters solvent layer or alkane solvents layer add salt solution, stir; Then the brine layer of lower floor is told in standing demix or centrifugal layering; The massfraction of salt solution is 3 ‰, and every kilogram of oleoresin capsicum adds 3～5L salt solution;
(5) divide the esters solvent layer behind the water layer that desalts or the alkane solvents layer is concentrated and desolvation is residual, can obtain removing the oleoresin capsicum of rhodamine B.
2. the removal method of rhodamine B in the oleoresin capsicum according to claim 1, it is characterized in that: in the described step (1), every kilogram of oleoresin capsicum is dissolved in 8～10L esters solvent or the alkane solvents.
3. the removal method of rhodamine B in the oleoresin capsicum according to claim 1 is characterized in that: in the described step (2), every kilogram of oleoresin capsicum adds 2～4L alcohol solution.
4. the removal method of rhodamine B in the oleoresin capsicum according to claim 1, it is characterized in that: the standing demix in the described step (3) is that mixed solution leaves standstill layering after 0.5～2 hour.
5. the removal method of rhodamine B in the oleoresin capsicum according to claim 1 is characterized in that: the standing demix in the described step (4) is for leaving standstill layering after 0.5～2 hour.
6. the removal method of rhodamine B in the described oleoresin capsicum of any one according to claim 1-5, it is characterized in that: described step (3) obtains the esters solvent layer or the alkane solvents layer is washed 4～5 times with alcohol solution according to step (2)-(3) again.
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| CN103740279B (en) * | 2013-12-25 | 2015-09-16 | 晨光生物科技集团股份有限公司 | Not containing the production method of the oleoresin capsicum of aflatoxin |
| CN106590436A (en) * | 2016-12-27 | 2017-04-26 | 晨光生物科技集团股份有限公司 | Production process for removing rhodamine B in capsicum oleoresin |
| CN107236461A (en) * | 2017-06-05 | 2017-10-10 | 青岛红星化工集团天然色素有限公司 | The minimizing technology of Hostathion in a kind of capsicum oleoresin |
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| CN1155561C (en) * | 2000-11-29 | 2004-06-30 | 贵州五倍子发展有限公司 | Process for preparing capsicine compounds from capsicol resin |
| CN100494976C (en) * | 2007-04-17 | 2009-06-03 | 广东省疾病预防控制中心 | Method for detecting fat-soluble azo dyes in food or fodder and its kit |
| CN101733082A (en) * | 2009-12-28 | 2010-06-16 | 嘉兴学院 | Method for preparing rhodamine B molecular engram solid phase extraction stuffing and application thereof |
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