CN103740279B - Not containing the production method of the oleoresin capsicum of aflatoxin - Google Patents
Not containing the production method of the oleoresin capsicum of aflatoxin Download PDFInfo
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- CN103740279B CN103740279B CN201310725060.5A CN201310725060A CN103740279B CN 103740279 B CN103740279 B CN 103740279B CN 201310725060 A CN201310725060 A CN 201310725060A CN 103740279 B CN103740279 B CN 103740279B
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Abstract
The invention discloses a kind of not containing the production method of the oleoresin capsicum of aflatoxin, its processing step is: 1) extracted by capsicum crude extract alcohol water mixed solvent, is separated, obtains resin extracting solution; 2) organic solvent in deresinate extracting solution, then adds alkane solvents and dissolves, obtain resin solution; 3) in resin solution, add alkali aqueous solution and carry out agitator treating, be separated and remove aqueous phase, obtain alkali cleaning organic phase; 4) in alkali cleaning organic phase, add aqueous acid and carry out agitator treating, be again separated and remove aqueous phase, obtain pickling organic phase; 5) pickling organic phase salt brine solution is carried out agitator treating, be separated and remove aqueous phase; The salt obtained is washed organic phase desolvation and is remained, and can obtain not containing the oleoresin capsicum of aflatoxin.Present method utilizes the difference of capsaicine and aflatoxin characteristic, have capsaicine yield high while, can obtain, not containing the oleoresin capsicum of aflatoxin, there is the reliable feature of product safety.
Description
Technical field
The present invention relates to a kind of production method of oleoresin capsicum, especially a kind of not containing the production method of the oleoresin capsicum of aflatoxin.
Background technology
Aflatoxin (aflatoxin is called for short AFT) is the toxicity secondary metabolic product that a class is produced by flavus Aspergillus parasiticus etc., is to one of larger mycotoxins of human and animal's harm.Great mass of data confirms, the liver organization of aflatoxin to people and animal has very strong toxic action, can cause liver cancer time serious, even dead.Wherein aflatoxin B1 is most in the world strong carcinogen known at present, is classified as 1A class carcinogens by WHO, very harmful to the mankind.
Capsicum is as most important sharp flavor seasoning good merchantable brand, indispensable in food-processing.Capsicum in storage process due to the multiple reasons such as weather, environment, situation about polluting by flavus also more easily occurs, oleoresin capsicum is a kind of oily liquids extracted from capsicum, remain the strong sharp flavor of capsicum, and there is pungency component quantification, stdn, easy to use, low cost and other advantages, replace capsicum to be widely used in the industry such as food, seasonings in a large number.And Fructus Capsici extract is in process of production due to Extraction and enrichment effect, cause aflatoxin to obtain enrichment in oleoresin capsicum, produce and pollute.
The oleoresin capsicum of China has occupied about 40% of international market share, but up to now, there is no the open report removing aflatoxin in oleoresin capsicum, develop so a kind of technique, comply with food safety development situation on the one hand, on the other hand by improving Product Safety, the synthesized competitiveness of product can be strengthened, to raising international market share, there is very large realistic meaning.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of not containing the production method of the oleoresin capsicum of aflatoxin, with the pollution effectively avoiding oleoresin capsicum to suffer aflatoxin.
For solving the problems of the technologies described above, the processing step that the present invention takes is: capsicum crude extract alcohol water mixed solvent extracts by (1), is separated, obtains resin extracting solution;
(2) organic solvent in deresinate extracting solution, then adds alkane solvents and dissolves, obtain resin solution;
(3) in resin solution, add alkali aqueous solution and carry out agitator treating, be separated and remove aqueous phase, obtain alkali cleaning organic phase;
(4) in alkali cleaning organic phase, add aqueous acid and carry out agitator treating, be again separated and remove aqueous phase, obtain pickling organic phase;
(5) pickling organic phase salt brine solution is carried out agitator treating, be separated and remove aqueous phase; The salt obtained is washed organic phase desolvation and is remained, and can obtain not containing the oleoresin capsicum of aflatoxin.
Alcohol water mixed solvent volume ratio in step of the present invention (1) is methanol-water and/or the ethanol water of 2:1 ~ 9:1.During described extraction, the mass volume ratio of feed liquid is 1:3 ~ 1:6, and Extracting temperature is 30 ~ 40 DEG C.
Alkane solvents in step of the present invention (2) is normal hexane, hexanaphthene or sherwood oil, and feed liquid mass volume ratio is 1:4 ~ 1:6.
Alkali aqueous solution in step of the present invention (3) is sodium hydroxide solution, potassium hydroxide solution or sodium carbonate solution, and the massfraction of solution is 2 ~ 5 ‰.The volume ratio of described resin solution and alkali lye is 1:1 ~ 1:4, at 30 ~ 50 DEG C stirs after adding alkali aqueous solution in organic phase.
Aqueous acid is hydrochloric acid, phosphoric acid or citric acid in step of the present invention (4), and massfraction is 2 ~ 5 ‰, and the material liquid volume used is than being 1:1 ~ 1:4.Stir at 30 ~ 50 DEG C after adding aqueous acid in described alkali cleaning organic phase.
The salt brine solution used in step of the present invention (5) is sodium chloride solution, and massfraction is 2 ~ 5 ‰.The volume ratio of described pickling organic phase and salt brine solution is 1:1 ~ 1:4, and agitator treating number of times is 2 ~ 3 times.
The present invention utilizes capsaicine and aflatoxin qualitative difference Transformatin aflatoxin, it removes principle: aflatoxin forms tonka bean camphor salt in alkaline solution, soluble in water, but solubleness is deteriorated in organic phase, aflatoxin is made to become the water-soluble removing of salt by soda lye wash, and most capsaicine is stayed in alkane solvents, a part of water-soluble impurity in oleoresin capsicum also can wash out by salt solution simultaneously, comprises in impurity the aflatoxin being wrapped with trace; Thus the oleoresin capsicum obtained is not containing aflatoxin.
The beneficial effect adopting technique scheme to produce is: the present invention makes full use of the difference of capsaicine and aflatoxin characteristic, in leaching process capsaicine yield high while, can obtain, not containing the oleoresin capsicum of the high security of aflatoxin, there is the reliable feature of product safety.Present invention process is simple, process safety is high, easy to operate, and can suitability for industrialized production be realized.
Embodiment
Below in conjunction with specific embodiment, the present invention is further detailed explanation.
Embodiment 1: the production technique not containing the oleoresin capsicum of aflatoxin adopts following processing step.
(1) add aflatoxin B1, B2, G1, G2 standard model in capsicum crude extract, capsaicin content is 8wt% after testing, and Aflatoxin B1,B2,G1 and G2 content is 50,8.8,9.0 and 7.1ug/kg.Sampling 30kg adds the ethanol water of 90L, and ethanol: water=3:1 (volume), stirs extraction 3 times at 40 DEG C, and centrifugal merging supernatant liquor, obtains resin extracting solution;
(2) above-mentioned resin extracting solution is carried out desolventizing in thin-film evaporator, slough most solvent; Normal hexane is added, enriched material: normal hexane=1:4(kg/l in enriched material after precipitation), stirring and dissolving, obtains resin solution;
(3) in resin solution, the aqueous sodium hydroxide solution of massfraction 3 ‰ is added, resin solution: aqueous sodium hydroxide solution=1:2(volume), stir at 30 DEG C and make it mix, leave standstill 30min, layering, removing water layer, obtains alkali cleaning organic layer (alkali cleaning organic phase);
(4) in above-mentioned alkali cleaning organic layer, the aqueous hydrochloric acid of massfraction 4 ‰ is added, alkali cleaning organic layer: aqueous hydrochloric acid=1:2(volume), be uniformly mixed at 30 DEG C, after leaving standstill 30min, layering, removing water layer, obtains pickling organic layer (pickling organic phase);
(5) in above-mentioned pickling organic layer, the common salt aqueous solution of massfraction 2 ‰ is added, pickling organic layer: common salt aqueous solution=1:2(volume), stir 30min; Standing 30min carries out layering and removes water layer; Repeat salt and wash and remove water layer process 3 times, obtain salt and wash organic layer (organic phase washed by salt);
(6) salt will be obtained wash organic layer vacuum and take off taste pot and carry out concentrated desolvation and remain, obtain oleoresin capsicum 2.91kg, capsaicin content is 78wt%, capsaicine yield is 95%, use the AFT content in immune affinity column-post-column derivation-liquid chromatography fluorescence detector testing product, result does not detect.
Embodiment 2: the production technique not containing the oleoresin capsicum of aflatoxin adopts following processing step.
(1) add aflatoxin B1, B2, G1, G2 standard model in capsicum crude extract, capsaicin content is 8% after testing, and Aflatoxin B1,B2,G1 and G2 content is 50,8.8,9.0 and 7.1ug/kg.Sampling 30kg adds the methanol-water of 150L, volume ratio 6:1, and at 40 DEG C, stir extraction 3 times, centrifugal merging supernatant liquor, obtains resin extracting solution;
(2) above-mentioned resin extracting solution is carried out desolventizing in thin-film evaporator, in enriched material, add the hexanaphthene of mass volume ratio 1:5, stirring and dissolving, obtain resin solution;
(3) in above-mentioned resin solution, add the potassium hydroxide aqueous solution of massfraction 5 ‰ according to volume ratio 1:3, stir at 30 DEG C and make it mix, obtain mixed solution; Leave standstill 30min, layering, removing water layer, obtains alkali cleaning organic layer;
(4) in above-mentioned alkali cleaning organic layer, add the phosphate aqueous solution of massfraction 3 ‰ according to volume ratio 1:4, be constantly uniformly mixed at 30 DEG C, after leaving standstill 30min, layering, removing water layer, obtains pickling organic layer;
(5) in above-mentioned pickling organic layer, add the common salt aqueous solution of massfraction 3 ‰ according to volume ratio 1:1, stir 60min; Leave standstill 30min layering, remove water layer; Repeat that above-mentioned salt is washed, layer process of anhydrating 2 times, obtain salt and wash organic layer;
(6) salt is washed organic layer concentrating under reduced pressure desolvation to remain, obtain oleoresin capsicum 3.11kg, capsaicin content is 76wt%, and capsaicine yield is 98%, use the AFT content in immune affinity column-post-column derivation-liquid chromatography fluorescence detector testing product, result does not detect.
Embodiment 3: the production technique not containing the oleoresin capsicum of aflatoxin adopts following processing step.
(1) add aflatoxin B1, B2, G1, G2 standard model in capsicum crude extract, capsaicin content is 8% after testing, and Aflatoxin B1,B2,G1 and G2 content is 50,8.8,9.0 and 7.1ug/kg.Sampling 30kg adds the methanol-water of 120L, volume ratio 9:1, and at 35 DEG C, stir extraction 3 times, centrifugal merging supernatant liquor, obtains resin extracting solution;
(2) above-mentioned resin extracting solution is carried out desolventizing in thin-film evaporator, in enriched material, add the sherwood oil of mass volume ratio 1:6, stirring and dissolving, obtain resin solution;
(3) in above-mentioned resin solution, add the aqueous sodium carbonate of massfraction 4 ‰ according to volume ratio 1:1, at 40 DEG C, stir 30min make it mix, obtain mixed solution, leave standstill 40min layering, lower floor is removed, obtains alkali cleaning organic layer;
(4) in alkali cleaning organic layer, add the aqueous citric acid solution of massfraction 2 ‰ according to volume ratio 1:4, at 40 DEG C, be constantly uniformly mixed 60min; Leave standstill 40min layering, remove water layer, obtain pickling organic layer;
(5) in above-mentioned pickling organic layer, add the common salt aqueous solution of massfraction 4 ‰ according to volume ratio 1:3, stir 60min; Leave standstill 30min layering, remove water layer; Repeat above-mentioned salt and wash and remove water layer process 3 times, obtain salt and wash organic layer.
(6) salt obtained is washed organic layer concentrating under reduced pressure desolvation to remain, obtain oleoresin capsicum 2.76kg, capsaicin content is 80wt%, and capsaicine yield is 92%, use the AFT content in immune affinity column-post-column derivation-liquid chromatography fluorescence detector testing product, result does not detect.
Embodiment 4: the production technique not containing the oleoresin capsicum of aflatoxin adopts following processing step.
(1) add aflatoxin B1, B2, G1, G2 standard model in capsicum crude extract, capsaicin content is 8% after testing, and Aflatoxin B1,B2,G1 and G2 content is 50,8.8,9.0 and 7.1ug/kg.Sampling 30kg adds the methanol-water of 180L, volume ratio 2:1, and at 30 DEG C, stir extraction 3 times, centrifugal merging supernatant liquor, obtains resin extracting solution;
(2) above-mentioned resin extracting solution is carried out desolventizing in thin-film evaporator, in enriched material, add the hexanaphthene of mass volume ratio 1:5, stirring and dissolving, obtain resin solution;
(3) in above-mentioned resin solution, add the potassium hydroxide aqueous solution of massfraction 2 ‰ according to volume ratio 1:4, stir at 50 DEG C and make it mix, obtain mixed solution; Leave standstill 30min, layering, removing water layer, obtains alkali cleaning organic layer;
(4) in above-mentioned alkali cleaning organic layer, add the aqueous citric acid solution of massfraction 5 ‰ according to volume ratio 1:1, be constantly uniformly mixed at 50 DEG C, after leaving standstill 30min, layering, removing water layer, obtains pickling organic layer;
(5) in above-mentioned pickling organic layer, add the common salt aqueous solution of massfraction 5 ‰ according to volume ratio 1:4, stir 60min; Leave standstill 30min layering, remove water layer; Repeat that above-mentioned salt is washed, layer process of anhydrating 2 times, obtain salt and wash organic layer;
(6) salt is washed organic layer concentrating under reduced pressure desolvation to remain, obtain oleoresin capsicum 2.98kg, capsaicin content is 77wt%, and capsaicine yield is 97%, use the AFT content in immune affinity column-post-column derivation-liquid chromatography fluorescence detector testing product, result does not detect.
Claims (9)
1. one kind does not contain the production method of the oleoresin capsicum of aflatoxin, it is characterized in that, the processing step of the method is: capsicum crude extract alcohol water mixed solvent extracts by (1), be separated, obtain resin extracting solution, alcohol water mixed solvent volume ratio is methanol-water and/or the ethanol water of 2:1 ~ 9:1;
(2) organic solvent in deresinate extracting solution, then adds alkane solvents and dissolves, obtain resin solution;
(3) in resin solution, add alkali aqueous solution and carry out agitator treating, be separated and remove aqueous phase, obtain alkali cleaning organic phase;
(4) in alkali cleaning organic phase, add aqueous acid and carry out agitator treating, be again separated and remove aqueous phase, obtain pickling organic phase;
(5) pickling organic phase salt brine solution is carried out agitator treating, be separated and remove aqueous phase; The salt obtained is washed organic phase desolvation and is remained, and can obtain not containing the oleoresin capsicum of aflatoxin.
2. according to claim 1 not containing the production method of the oleoresin capsicum of aflatoxin, it is characterized in that: during described extraction, the mass volume ratio of feed liquid is 1:3 ~ 1:6 kg/L, and Extracting temperature is 30 ~ 40 DEG C.
3., according to the production method not containing the oleoresin capsicum of aflatoxin described in claim 1, it is characterized in that: the alkane solvents in described step (2) is normal hexane, hexanaphthene or sherwood oil, feed liquid mass volume ratio is 1:4 ~ 1:6 kg/L.
4. according to the production method not containing the oleoresin capsicum of aflatoxin described in claim 1, it is characterized in that: the alkali aqueous solution in described step (3) is sodium hydroxide solution, potassium hydroxide solution or sodium carbonate solution, the massfraction of solution is 2 ~ 5 ‰.
5., according to the production method not containing the oleoresin capsicum of aflatoxin described in claim 4, it is characterized in that: the volume ratio of described resin solution and alkali aqueous solution is 1:1 ~ 1:4, at 30 ~ 50 DEG C stirs after adding alkali aqueous solution in organic phase.
6. according to the production method not containing the oleoresin capsicum of aflatoxin described in claim 1, it is characterized in that: in described step (4), aqueous acid is hydrochloric acid, phosphoric acid or citric acid, massfraction is 2 ~ 5 ‰, and the material liquid volume used is than being 1:1 ~ 1:4.
7., according to the production method not containing the oleoresin capsicum of aflatoxin described in claim 6, it is characterized in that: stir at 30 ~ 50 DEG C after adding aqueous acid in described alkali cleaning organic phase.
8. the production method not containing the oleoresin capsicum of aflatoxin according to claim 1-7 any one, it is characterized in that: the salt brine solution used in described step (5) is sodium chloride solution, massfraction is 2 ~ 5 ‰.
9. the production method not containing the oleoresin capsicum of aflatoxin described according to Claim 8, is characterized in that: the volume ratio of described pickling organic phase and salt brine solution is 1:1 ~ 1:4, and agitator treating number of times is 2 ~ 3 times.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102433072A (en) * | 2011-09-22 | 2012-05-02 | 晨光生物科技集团股份有限公司 | Method for removing rhodamine B in capsicum oleoresin |
| CN102746793A (en) * | 2012-07-31 | 2012-10-24 | 云南宏绿辣素有限公司 | Method for refining capsicum oleoresins |
| CN102987225A (en) * | 2012-11-22 | 2013-03-27 | 江南大学 | Method for removing aflatoxin in rice flour |
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| JPS5934736B2 (en) * | 1979-07-10 | 1984-08-24 | 長谷川香料株式会社 | Manufacturing method of paprika pigment |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102433072A (en) * | 2011-09-22 | 2012-05-02 | 晨光生物科技集团股份有限公司 | Method for removing rhodamine B in capsicum oleoresin |
| CN102746793A (en) * | 2012-07-31 | 2012-10-24 | 云南宏绿辣素有限公司 | Method for refining capsicum oleoresins |
| CN102987225A (en) * | 2012-11-22 | 2013-03-27 | 江南大学 | Method for removing aflatoxin in rice flour |
Non-Patent Citations (1)
| Title |
|---|
| 食品中黄曲霉毒素及理化脱毒措施研究进展;刘罗发等;《安徽农业科学》;20111231;第39卷(第8期);第4756-4757、4759页 * |
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