CN103694728B - Method for removing 4-methylimidazole in caramel pigment - Google Patents
Method for removing 4-methylimidazole in caramel pigment Download PDFInfo
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- CN103694728B CN103694728B CN201310702045.9A CN201310702045A CN103694728B CN 103694728 B CN103694728 B CN 103694728B CN 201310702045 A CN201310702045 A CN 201310702045A CN 103694728 B CN103694728 B CN 103694728B
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- Prior art keywords
- methylimidazole
- caramel colorant
- caramel
- adsorption
- caramel pigment
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- XLSZMDLNRCVEIJ-UHFFFAOYSA-N 4-methylimidazole Chemical compound CC1=CNC=N1 XLSZMDLNRCVEIJ-UHFFFAOYSA-N 0.000 title claims abstract description 70
- MIDXCONKKJTLDX-UHFFFAOYSA-N 3,5-dimethylcyclopentane-1,2-dione Chemical compound CC1CC(C)C(=O)C1=O MIDXCONKKJTLDX-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 235000013736 caramel Nutrition 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000000049 pigment Substances 0.000 title abstract description 8
- 238000001179 sorption measurement Methods 0.000 claims abstract description 31
- 230000001105 regulatory effect Effects 0.000 claims abstract description 6
- 239000003086 colorant Substances 0.000 claims description 46
- 239000000243 solution Substances 0.000 claims description 16
- 239000008186 active pharmaceutical agent Substances 0.000 claims description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims description 9
- 239000010935 stainless steel Substances 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 14
- 235000013305 food Nutrition 0.000 abstract description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 4
- 229910021529 ammonia Inorganic materials 0.000 abstract description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 239000000940 FEMA 2235 Substances 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 6
- 239000012530 fluid Substances 0.000 description 6
- 238000005304 joining Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 239000001117 sulphuric acid Substances 0.000 description 6
- 235000011149 sulphuric acid Nutrition 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 239000004278 EU approved seasoning Substances 0.000 description 2
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 235000011194 food seasoning agent Nutrition 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005374 membrane filtration Methods 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 229920000856 Amylose Polymers 0.000 description 1
- 206010010904 Convulsion Diseases 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 241000699666 Mus <mouse, genus> Species 0.000 description 1
- 241000699670 Mus sp. Species 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 235000012970 cakes Nutrition 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 230000036461 convulsion Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000000576 food coloring agent Substances 0.000 description 1
- 235000002864 food coloring agent Nutrition 0.000 description 1
- 239000000989 food dye Substances 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000014347 soups Nutrition 0.000 description 1
- 235000013555 soy sauce Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- 235000021419 vinegar Nutrition 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a method for removing 4-methylimidazole in a caramel pigment. The method comprises the steps of: preparing into a water solution by using the caramel pigment, regulating the brix and a pH value, placing in an electric adsorption device, and applying a voltage for electrically adsorbing to remove 4-methylimidazole. According to the method, the technical difficulty that the content of 4-methylimidazole in the caramel pigment of an ammonia process exceeds the standard is effectively solved, and the quality and the food safety of the caramel pigment product are improved. Compared with a currently common treatment technology, the method disclosed by the invention has the advantages of simplicity and convenience in operation, low cost and the like, and can be performed repeatedly.
Description
Technical field
The invention belongs to technical field of food additives, particularly a kind of method removing 4-methylimidazole in caramel colorant.
Background technology
Pigment can increase the organoleptic property of food, improves the commodity value of food, and therefore application is in the industry more and more extensive.Caramel colorant, also claims dark reddish brown, and food color market occupies an important position, and is the foodstuff additive that current Applications in Food Industry is widest in area, quantity is maximum, is widely used in the industries such as seasonings, food, beverage, medicine.Caramel colorant be with the sucrose of high-quality, glucose or other β-amylose for main raw material, adopt the natural pigment that special formula and Technology are processed into.Caramel colorant has the features such as good water solubility, strong coloring force, stable in properties, safety non-toxic, is that in current food dye, consumption is maximum, use range is the widest, using it as a kind of pigment that the country of food colorant is maximum.
According to the classification of international technology caramel colorant association (ITCA), ammonium (ammonia) method caramel refers in the course of processing not containing sulphite only adopts ammonia or ammonium salt to make as a catalyzer class caramel colorant as catalyzer, its use range is wider, be mainly used in brewageing seasonings and the Medicines and Health Product such as (as soy sauce, jam product, spiced and stewed food, vinegar), beer, candy, cake, soup stock, usually positively charged.
Ammonium (ammonia) method caramel is owing to can produce a certain amount of 4-methylimidazole (C in process of production
4h
6n
2), cause 4-methylimidazole content overproof in the caramel colorant sample prepared.4-methylimidazole is Nervous toxicity, can cause convulsions, and US Experts also by tests on white mice, determines that it exceedes certain content and has carcinogenic effect to white mouse.The consciousness of people to food safety is more and more higher, the enterprise producing caramel colorant is in recent years impelled all to compare the control focused on 4-methylimidazole content in process of production, some large factory domestic and more external producer adopt membrane filtration technique to process the caramel colorant sample produced at present, to reach impurity such as removing 4-methylimidazole, the object of improving the quality of products.But membrane filtration technique cost is high, complicated operation, the pressure that enterprise applies this technology is large, is difficult to be promoted use.
Summary of the invention
The object of the invention is to the deficiency of client's prior art, a kind of method removing 4-methylimidazole in caramel colorant is provided.
The technical solution used in the present invention is:
Remove a method for 4-methylimidazole in caramel colorant, adopt the 4-methylimidazole in electro-adsorption method removal caramel colorant sample.
Preferably, comprise the following steps: prepare the caramel colorant aqueous solution, after regulating brix to 50 ~ 65 ° Bx, be placed in electric adsorption device, apply voltage, carry out electro-adsorption.
Preferably, caramel colorant aqueous solution pH to 3.0 ~ 4.5 are regulated.
Preferably, adsorb under volts DS 4 ~ 6v.
Preferably, adsorption time is 3 ~ 6h.
Preferably, in adsorption process, with the speed stirring solution of 50 ~ 100rpm.
Preferably, using stainless steel plate as anode.
The invention has the beneficial effects as follows:
The present invention adopts the 4-methylimidazole in electro-adsorption method removal caramel colorant sample, efficiently solves the technical barrier that ammonium method caramel colorant 4-methylimidazole exceeds standard, improves quality and the edible safety of caramel colorant product.The inventive method compared with at present conventional treatment technology, have simple to operation, can repeat, low cost and other advantages.
Embodiment
In the preparation process of ammonium method caramel colorant, because material and ammonium salt can produce a kind of Nervous toxicity at a certain temperature---4-methylimidazole, as misoperation is easy to the caramel colorant sample 4-methylimidazole content overproof that causes preparing.Have the structure of conjugatedπbond and lone-pair electron according to 4-methylimidazole, π-electron is easily adsorbed on the feature of electrode surface, and the present invention adopts the 4-methylimidazole in the method for electro-adsorption ingenious removal caramel colorant sample.
The present invention removes the method for 4-methylimidazole in caramel colorant, comprises the following steps: prepare the caramel colorant aqueous solution, after regulating brix to 50 ~ 65 ° Bx, is placed in electric adsorption device, applies voltage, carries out electro-adsorption.
Preferably, caramel colorant aqueous solution pH to 3.0 ~ 4.5 are regulated.
Preferably, adsorb under volts DS 4 ~ 6v.
Preferably, adsorption time is 3 ~ 6h.
Preferably, in adsorption process, with the speed stirring solution of 50 ~ 100rpm.
Preferably, using stainless steel plate as anode.
After absorption terminates, the content of 4-methylimidazole in working sample, can repeat electro-adsorption, until 4-methylimidazole content reaches the requirement of setting in caramel colorant sample.
Below in conjunction with specific embodiment, set forth content of the present invention further.
embodiment 1
The step removing 4-methylimidazole in caramel colorant sample is as follows:
(1) get with the standby caramel colorant sample of ammonium legal system, be dissolved in water and regulate brix to 50 ° Bx, regulate pH to be 3.0 with dilute sulphuric acid;
(2) caramel color solution is placed in electric adsorption device (positive pole and stainless steel plate connect and compose anode, and negative pole and joining of graphite form negative electrode), control volts DS is 4v, carry out electro-adsorption, simultaneously with 50rpm low rate mixing solution, after absorption 6h, powered-down.By for subsequent use after the dilute hydrochloric acid cleaning of the anode 0.1mol/L of absorption 4-methylimidazole, and reclaim washing fluid; Negative electrode water is for subsequent use after rinsing.
embodiment 2
The step removing 4-methylimidazole in caramel colorant sample is as follows:
(1) get with the standby caramel colorant sample of ammonium legal system, be dissolved in water and regulate brix to 55 ° Bx, regulate pH to be 3.0 with dilute sulphuric acid;
(2) (positive pole and stainless steel plate connect and compose anode caramel color solution to be placed in electric adsorption device, negative pole and joining of graphite form negative electrode), control volts DS is 6v, carry out electro-adsorption, simultaneously with 50rpm low rate mixing solution, after absorption 3h, powered-down, for subsequent use after the dilute hydrochloric acid cleaning of anode 0.1mol/L, and reclaim washing fluid; Negative electrode water is for subsequent use after rinsing.
embodiment 3
The step removing 4-methylimidazole in caramel colorant sample is as follows:
(1) get with the standby caramel colorant sample of ammonium legal system, be dissolved in water and regulate brix to 60 ° Bx, regulate pH to be 3.5 with dilute sulphuric acid;
(2) (positive pole and stainless steel plate connect and compose anode caramel color solution to be placed in electric adsorption device, negative pole and joining of graphite form negative electrode), control volts DS is 5v, carry out electro-adsorption, simultaneously with 80rpm low rate mixing solution, after absorption 6h, powered-down, for subsequent use after the dilute hydrochloric acid cleaning of anode 0.1mol/L, and reclaim washing fluid; Negative electrode water is for subsequent use after rinsing.
embodiment 4
The step removing 4-methylimidazole in caramel colorant sample is as follows:
(1) get with the standby caramel colorant sample of ammonium legal system, be dissolved in water and regulate brix to 60 ° Bx, regulate pH to be 3.5 with dilute sulphuric acid;
(2) (positive pole and stainless steel plate connect and compose anode caramel color solution to be placed in electric adsorption device, negative pole and joining of graphite form negative electrode), control volts DS is 6v, carry out electro-adsorption, simultaneously with 80rpm low rate mixing solution, after absorption 3h, powered-down, for subsequent use after the dilute hydrochloric acid cleaning of anode 0.1mol/L, and reclaim washing fluid; Negative electrode water is for subsequent use after rinsing.
embodiment 5
The step removing 4-methylimidazole in caramel colorant sample is as follows:
(1) get with the standby caramel colorant sample of ammonium legal system, be dissolved in water and regulate brix to 65 ° Bx, regulate pH to be 4.0 with dilute sulphuric acid;
(2) (positive pole and stainless steel plate connect and compose anode caramel color solution to be placed in electric adsorption device, negative pole and joining of graphite form negative electrode), control volts DS is 4v, carry out electro-adsorption, simultaneously with 100rpm low rate mixing solution, after absorption 6h, powered-down, for subsequent use after the dilute hydrochloric acid cleaning of anode 0.1mol/L, and reclaim washing fluid; Negative electrode water is for subsequent use after rinsing.
embodiment 6
The step removing 4-methylimidazole in caramel colorant sample is as follows:
(1) get with the standby caramel colorant sample of ammonium legal system, be dissolved in water and regulate brix to 65 ° Bx, regulate pH to be 4.5 with dilute sulphuric acid;
(2) (positive pole and stainless steel plate connect and compose anode caramel color solution to be placed in electric adsorption device, negative pole and joining of graphite form negative electrode), control volts DS is 6v, carry out electro-adsorption, simultaneously with 100rpm low rate mixing solution, after absorption 3h, powered-down, for subsequent use after the dilute hydrochloric acid cleaning of anode 0.1mol/L, and reclaim washing fluid; Negative electrode water is for subsequent use after rinsing.
Caramel colorant sample electro-adsorption treatment effect is analyzed as follows shown in table:
All the other physical and chemical indexs meet GB8817-2001 national standard.
Claims (5)
1. remove the method for 4-methylimidazole in caramel colorant for one kind, it is characterized in that: adopt the 4-methylimidazole in electro-adsorption method removal caramel colorant sample, comprise the following steps: prepare the caramel colorant aqueous solution, regulate caramel colorant aqueous solution pH to 3.0 ~ 4.5, after regulating brix to 50 ~ 65 ° Bx, be placed in electric adsorption device, apply voltage, carry out electro-adsorption.
2. the method for 4-methylimidazole in removal caramel colorant according to claim 1, is characterized in that: adsorb under volts DS 4 ~ 6v.
3. the method for 4-methylimidazole in removal caramel colorant according to claim 1 and 2, is characterized in that: adsorption time is 3 ~ 6h.
4. the method for 4-methylimidazole in removal caramel colorant according to claim 1, is characterized in that: in adsorption process, with the speed stirring solution of 50 ~ 100rpm.
5. the method for 4-methylimidazole in removal caramel colorant according to claim 1, is characterized in that: using stainless steel plate as anode.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310702045.9A CN103694728B (en) | 2013-12-19 | 2013-12-19 | Method for removing 4-methylimidazole in caramel pigment |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310702045.9A CN103694728B (en) | 2013-12-19 | 2013-12-19 | Method for removing 4-methylimidazole in caramel pigment |
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| Publication Number | Publication Date |
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| CN103694728A CN103694728A (en) | 2014-04-02 |
| CN103694728B true CN103694728B (en) | 2015-02-25 |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108559303A (en) * | 2018-04-24 | 2018-09-21 | 肇庆焕发生物科技有限公司 | A kind of method of tetramethyl imidazoles in reduction caramel colorant |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4614662A (en) * | 1985-08-26 | 1986-09-30 | D. D. Williamson & Co., Inc. | Fast cook-continuous process for production of ammonia caramel color |
| CN102643862A (en) * | 2012-04-06 | 2012-08-22 | 千禾味业食品股份有限公司 | Method for producing high-safety caramel color through twice catalytic reaction |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110244102A1 (en) * | 2010-03-30 | 2011-10-06 | Pepsico, Inc. | Removal Of Reaction Byproducts And Impurities From Caramel Color And A Shelf Stable Caramel Color Concentrate |
-
2013
- 2013-12-19 CN CN201310702045.9A patent/CN103694728B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4614662A (en) * | 1985-08-26 | 1986-09-30 | D. D. Williamson & Co., Inc. | Fast cook-continuous process for production of ammonia caramel color |
| CN102643862A (en) * | 2012-04-06 | 2012-08-22 | 千禾味业食品股份有限公司 | Method for producing high-safety caramel color through twice catalytic reaction |
Non-Patent Citations (3)
| Title |
|---|
| "低4-甲基咪唑含量的焦糖色素制备工艺的研究";谭文兴 等;《甘蔗糖业》;20131215(第6期);23-28 * |
| "电吸附对水中盐类、氨氮、COD的去除效果分析";崔馨心 等;《环境工程学报》;20131205;第7卷(第12期);4805-4810 * |
| "电吸附技术的应用与研究";陈榕 等;《化学进展》;20060131;第18卷(第1期);80-86 * |
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Inventor after: Tan Wenxing Inventor after: Chang Guowei Inventor after: Li Zhide Inventor after: Zhao Biqiu Inventor after: Liang Dafeng Inventor after: Deng Guanghua Inventor after: Huang Yunan Inventor after: Nong Lizhong Inventor after: Zhong Yingping Inventor after: Yi Ximiao Inventor after: Li Yuhong Inventor before: Tan Wenxing Inventor before: Chang Guowei Inventor before: Li Zhide Inventor before: Zhao Biqiu Inventor before: Liang Dafeng Inventor before: Deng Guanghua Inventor before: Huang Yunan Inventor before: Nong Lizhong Inventor before: Zhong Yingping Inventor before: Yi Ximiao Inventor before: Li Yuhong |
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Effective date of registration: 20170527 Address after: 510316 Haizhuqu District, Guangdong Province, No. ten, road Co-patentee after: Guangzhou Hua Sugar Food Co., Ltd. Patentee after: Guangzhou Sugarcane Industry Research Institute Address before: 510316 Haizhuqu District, Guangdong Province, No. ten, road Co-patentee before: Gaungzhou Huaqiao Sugar Factory Patentee before: Guangzhou Sugarcane Industry Research Institute |
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Address after: 510316 Haizhuqu District, Guangdong Province, No. ten, road Co-patentee after: Guangzhou Hua Sugar Food Co., Ltd. Patentee after: Guangdong Province Institute of Biological Engineering (Guangzhou Sugarcane Industry Research Institute) Address before: 510316 Haizhuqu District, Guangdong Province, No. ten, road Co-patentee before: Guangzhou Hua Sugar Food Co., Ltd. Patentee before: Guangzhou Sugarcane Industry Research Institute |
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Granted publication date: 20150225 Termination date: 20191219 |