CN103740129A - Preparation process of low 4-methylimidazole caramel pigment - Google Patents
Preparation process of low 4-methylimidazole caramel pigment Download PDFInfo
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Abstract
The invention discloses a preparation process of low 4-methylimidazole caramel pigment, wherein an ammonium carbonate catalyst is added step by step, the reaction temperature and reaction time are controlled strictly, a caramel reaction is carried out stage by stage, the prepared caramel pigment has a bright red color (the haematochrome index is higher than 5.5), the 4-methylimidazole content is low (smaller than 100 ppm), and all the physical and chemical indexes reach the GB8817-2001 national standard.
Description
Technical field
The invention belongs to the production technical field of food colorant, particularly a kind of preparation technology of low 4-methylimidazole caramel colorant.
Background technology
Caramel is commonly called as dark reddish brown, that a kind of dense sorrel is with the colloidalmaterial of special burnt odor taste, its color and luster has the impact of acid and alkali, alkali, and uniform coloring, the characteristic such as fast light, heat-resisting, it is a kind of natural food colour of usage quantity maximum in foodstuffs industry, be widely used in beverage, soy sauce, yellow rice wine, aromatic vinegar, beer and part baked food, account for the more than 90% of whole food colorant market sales volume, wherein especially maximum with cola beverages consumption.
The preparation Chang Weiwu ammonia process of current caramel colorant, ammonium salt process, ammonia process, hydrogenation method technique etc.According to the classification of international technology caramel colorant association (ITCA), ammonium (ammonia) method caramel refers to and in the course of processing, does not use a class caramel colorant that only adopts ammonia or ammonium salt to make as catalyzer as catalyzer containing sulphite, its use range is wider, be mainly used in brewageing seasonings and the Medicines and Health Products such as (as soy sauce, jam product, spiced and stewed food, vinegar), beer, candy, cake, soup stock, conventionally positively charged.Yet owing to can produce eclamptogenic 4-methylimidazole in this preparation process, the edible safety of ammonium (ammonia) method caramel colorant enjoys query.
Ammonium (ammonia) method caramel reaction mechanism is very complicated, the quality of the difference meeting remarkably influenced caramel colorant of processing condition.The traditional technology of current domestic ammonium (ammonia) method caramel is mainly: saccharic (amylum hydrolysate of the sugar or molasses clear liquid) is concentrated into relative density 1.33～1.38, and the ammonia that passes into liquid glucose amount 0.1% in the time of 140 ℃ is incubated several hours at 140 ℃; While being cooled to 90 ℃, discharging is filtered, and stores at 38 ℃.But the 4-methylimidazole content in the caramel colorant sample that this technique prepares nearly all surpasses national standard.Domestic some large factory and more external producers also adopt membrane filtration technique to process the caramel colorant sample of producing 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, operation more complicated, enterprise's applying pressure is large, is difficult to be promoted.Therefore how improving the preparation technology of traditional caramel colorant, make its 4-methylimidazole content reach national safety standard scope, is caramel colorant production industry problem demanding prompt solution.
Summary of the invention
The object of the invention is to overcome the deficiency of prior art, a kind of preparation technology of low 4-methylimidazole caramel colorant is provided.
The technical solution used in the present invention is:
A preparation technology for low 4-methylimidazole caramel colorant, comprises the following steps:
(1) after molasses are diluted by suitable quantity of water, sedimentation, gets pellucid syrup;
(2) liquid glucose is proceeded to reactor, add the sal volatile of liquid glucose quality 0.5～1%, control temperature at 115～120 ℃ of reaction 5～10min; Continue to add the sal volatile of liquid glucose quality 1～1.5%, control temperature at 120～122 ℃ of reaction 10～15min; Continue to add the sal volatile of liquid glucose quality 1.5～2.0%, control temperature at 122～125 ℃ of reaction 15～20min; Continue to add the sal volatile of liquid glucose quality 1～1.5%, control temperature at 120～122 ℃ of reaction 10～15min; Then control temperature at 115～120 ℃ of reaction 20～30min, finish reaction, obtain the caramel colorant of low 4-methylimidazole content.
Preferably, step (1), by after molasses dilutions, is warming up to 105～110 ℃ and maintain after 40～60min, is cooled to 60～80 ℃, carries out sedimentation.
Preferably, step (1), by molasses dilution, regulates behind pH to 1.5～2.8, heats up.
Preferably, step (1), gets after pellucid syrup, governor weight degree to 60～65 ° Bx.
Preferably, step (2), proceeds to reactor by liquid glucose, is warming up to after 115 ℃～120 ℃, adds sal volatile.
Preferably, sal volatile is saturated aqueous solution.
Preferably, step (2), finishes, after reaction, to be cooled to below 50 ℃.
Preferably, step (1), dilutes molasses and water by weight 1:0.2～0.25.
The invention has the beneficial effects as follows:
The present invention improves traditional ammonium method caramel colorant preparation technology, by add catalyzer in batches, the strict processing parameters such as temperature of reaction and time of controlling, carry out stage by stage caramel reaction, the caramel colorant color and luster scarlet (haematochrome index is more than 5.5) preparing, 4-methylimidazole low (being less than 100ppm), every physical and chemical index meets GB8817-2001 national standard.
Embodiment
Caramel reaction is a complicated process, except occurring Maillard reaction and caramelization, also have a lot of side reactions, wherein in the preparation of ammonium method caramel colorant, ammonium and reducing sugar can slowly generate 4-methylimidazole at a certain temperature, cause 4-methylimidazole content overproof in caramel colorant, and the formation of 4-methylimidazole there is close relationship with raw material, the temperature of reacting, time, pH etc.The present invention improves traditional ammonium method caramel colorant preparation technology, add catalyzer in batches, strict control temperature of reaction and time, carry out stage by stage caramel reaction, the caramel colorant color and luster scarlet (haematochrome index is more than 5.5) of preparation, 4-methylimidazole low (being less than 100ppm), every physical and chemical index meets GB8817-2001 national standard.
The preparation technology of the low 4-methylimidazole caramel colorant of the present invention, comprises the following steps:
(1) after molasses are diluted by suitable quantity of water, sedimentation, gets pellucid syrup;
(2) liquid glucose is proceeded to reactor, add the sal volatile of liquid glucose quality 0.5～1%, control temperature at 115～120 ℃ of reaction 5～10min; Continue to add the sal volatile of liquid glucose quality 1～1.5%, control temperature at 120～122 ℃ of reaction 10～15min; Continue to add the sal volatile of liquid glucose quality 1.5～2.0%, control temperature at 122～125 ℃ of reaction 15～20min; Continue to add the sal volatile of liquid glucose quality 1～1.5%, control temperature at 120～122 ℃ of reaction 10～15min; Then control temperature at 115～120 ℃ of reaction 20～30min, finish reaction, obtain the caramel colorant of low 4-methylimidazole content.
Preferably, step (1), by after molasses dilutions, is warming up to 105～110 ℃ and maintain after 40～60min, is cooled to 60～80 ℃, carries out sedimentation.
Preferably, step (1), by molasses dilution, regulates behind pH to 1.5～2.8, heats up.
Preferably, step (1), gets after pellucid syrup, governor weight degree to 60～65 ° Bx.
Preferably, step (2), proceeds to reactor by liquid glucose, is warming up to after 115 ℃～120 ℃, adds sal volatile, the time contacting, reduces the formation of 4-methylimidazole to reduce ammonium salt with liquid glucose.
Preferably, sal volatile is saturated aqueous solution.
Preferably, step (2), finishes, after reaction, to be cooled to below 50 ℃ in 5min.
Preferably, step (1), dilutes molasses and water by weight 1:0.2～0.25.
Preferably, step (2), adds the distilled water of liquid glucose quality 5～10%, and governor weight degree is also controlled temperature at 115～120 ℃ of reaction 20～30min, finishes reaction.
Below in conjunction with specific embodiment, further set forth content of the present invention.
embodiment 1
The preparation technology of low 4-methylimidazole caramel colorant:
(1) pre-treatment of molasses: get purified sugar molasses 4kg, add after water 1kg water dilution, add dilute sulphuric acid, regulating pH value is 1.5, is warming up to 105 ℃ and maintain 60min, is cooled to 80 ℃ of left and right and puts into slurry tank, gets pellucid syrup use after sedimentation;
(2) hammer degree regulates: add hammer degree to the 60 ° Bx of appropriate water adjusting liquid glucose, and pump is to reactor;
(3) step of reaction: first liquid glucose is rapidly heated to 115 ℃, then slowly drips the volatile salt saturated aqueous solution of liquid glucose quality 1%, control temperature at 115 ℃ of reaction 10min; Continue to drip the volatile salt saturated aqueous solution of liquid glucose quality 1%, control temperature at 120 ℃ of reaction 15min; Continue to drip the volatile salt saturated aqueous solution of liquid glucose quality 2.0%, control temperature at 122 ℃ of reaction 20min; Continue to drip the volatile salt saturated aqueous solution of liquid glucose quality 1.5%, control temperature at 120 ℃ of reaction 10min; Then drip distilled water and control temperature at 115 ℃ of reaction 20min;
(4) after reaction finishes, be depressed into finished pot, and in 5min, be cooled to below 50 ℃, obtain the caramel colorant of low 4-methylimidazole content.
embodiment 2
The preparation technology of low 4-methylimidazole caramel colorant:
(1) pre-treatment of molasses: get purified sugar molasses 5kg, add after water 1kg water dilution, add dilute sulphuric acid, regulating pH value is 2.0, is warming up to 105 ℃ and maintain 60min, is cooled to 60 ℃ of left and right and puts into slurry tank, gets pellucid syrup use after sedimentation;
(2) hammer degree regulates: add hammer degree to the 63 ° Bx of appropriate water adjusting liquid glucose, and pump is to reactor;
(3) step of reaction: first liquid glucose is rapidly heated to 120 ℃, then slowly drips the volatile salt saturated aqueous solution of liquid glucose quality 0.5%, control temperature at 120 ℃ of reaction 5min; Continue to drip the volatile salt saturated aqueous solution of liquid glucose quality 1%, control temperature at 122 ℃ of reaction 10min; Continue to drip the volatile salt saturated aqueous solution of liquid glucose quality 1.5%, control temperature at 125 ℃ of reaction 15min; Continue to drip the volatile salt saturated aqueous solution of liquid glucose quality 1%, control temperature at 122 ℃ of reaction 10min; Then drip distilled water and control temperature at 120 ℃ of reaction 20min;
(4) after reaction finishes, be depressed into finished pot, and in 5min, be cooled to below 50 ℃, obtain the caramel colorant of low 4-methylimidazole content.
embodiment 3
The preparation technology of low 4-methylimidazole caramel colorant:
(1) pre-treatment of molasses: get purified sugar molasses 4kg, add after water 1kg water dilution, add dilute sulphuric acid, regulating pH value is 2.0, is warming up to 110 ℃ and maintain 40min, is cooled to 80 ℃ of left and right and puts into slurry tank, gets pellucid syrup use after sedimentation;
(2) hammer degree regulates: add hammer degree to the 63 ° Bx of appropriate water adjusting liquid glucose, and pump is to reactor;
(3) step of reaction: first liquid glucose is rapidly heated to 118 ℃, then slowly drips the volatile salt saturated aqueous solution of liquid glucose quality 0.8%, control temperature at 118 ℃ of reaction 7min; Continue to drip the volatile salt saturated aqueous solution of liquid glucose quality 1.5%, control temperature at 120 ℃ of reaction 15min; Continue to drip the volatile salt saturated aqueous solution of liquid glucose quality 2.0%, control temperature at 122 ℃ of reaction 20min; Continue to drip the volatile salt saturated aqueous solution of liquid glucose quality 1.5%, control temperature at 120 ℃ of reaction 15min; Then drip distilled water and control temperature at 115 ℃ of reaction 30min;
(4) after reaction finishes, be depressed into finished pot, and in 5min, be cooled to below 50 ℃, obtain the caramel colorant of low 4-methylimidazole content.
embodiment 4
The preparation technology of low 4-methylimidazole caramel colorant:
(1) pre-treatment of molasses: get cane molasses 5kg, add after water 1kg water dilution, add dilute sulphuric acid, regulating pH value is 2.1, is warming up to 110 ℃ and maintain 40min, is cooled to 80 ℃ of left and right and puts into slurry tank, gets pellucid syrup use after sedimentation;
(2) hammer degree regulates: add hammer degree to the 64 ° Bx of appropriate water adjusting liquid glucose, and pump is to reactor;
(3) step of reaction: first liquid glucose is rapidly heated to 115 ℃, then slowly drips the volatile salt saturated aqueous solution of liquid glucose quality 1.0%, control temperature at 115 ℃ of reaction 10min; Continue to drip the volatile salt saturated aqueous solution of liquid glucose quality 1.5%, control temperature at 120 ℃ of reaction 15min; Continue to drip the volatile salt saturated aqueous solution of liquid glucose quality 2.0%, control temperature at 122 ℃ of reaction 20min; Continue to drip the volatile salt saturated aqueous solution of liquid glucose quality 1.5%, control temperature at 120 ℃ of reaction 15min; Then drip distilled water and control temperature at 115 ℃ of reaction 30min;
(4) after reaction finishes, be depressed into finished pot, and in 5min, be cooled to below 50 ℃, obtain the caramel colorant of low 4-methylimidazole content.
embodiment 5
The preparation technology of low 4-methylimidazole caramel colorant:
(1) pre-treatment of molasses: get cane molasses 4kg, add after water 1kg water dilution, add dilute sulphuric acid, regulating pH value is 2.1, is warming up to 105 ℃ and maintain 60min, is cooled to 70 ℃ of left and right and puts into slurry tank, gets pellucid syrup use after sedimentation;
(2) hammer degree regulates: add hammer degree to the 65 ° Bx of appropriate water adjusting liquid glucose, and pump is to reactor;
(3) step of reaction: first liquid glucose is rapidly heated to 115 ℃, then slowly drips the volatile salt saturated aqueous solution of liquid glucose quality 1.0%, control temperature at 115 ℃ of reaction 10min; Continue to drip the volatile salt saturated aqueous solution of liquid glucose quality 1.5%, control temperature at 120 ℃ of reaction 15min; Continue to drip the volatile salt saturated aqueous solution of liquid glucose quality 1.5%, control temperature at 125 ℃ of reaction 15min; Continue to drip the volatile salt saturated aqueous solution of liquid glucose quality 1%, control temperature at 122 ℃ of reaction 10min; Then drip distilled water and control temperature at 120 ℃ of reaction 20min;
(4) after reaction finishes, be depressed into finished pot, and in 5min, be cooled to below 50 ℃, obtain the caramel colorant of low 4-methylimidazole content.
Caramel colorant technical indicator prepared by the embodiment of the present invention is as shown in the table:
All the other physical and chemical indexs all meet GB8817-2001 national standard.
Claims (8)
1. a preparation technology for low 4-methylimidazole caramel colorant, comprises the following steps:
(1) after molasses are diluted by suitable quantity of water, sedimentation, gets pellucid syrup;
(2) liquid glucose is proceeded to reactor, add the sal volatile of liquid glucose quality 0.5～1%, control temperature at 115～120 ℃ of reaction 5～10min; Continue to add the sal volatile of liquid glucose quality 1～1.5%, control temperature at 120～122 ℃ of reaction 10～15min; Continue to add the sal volatile of liquid glucose quality 1.5～2.0%, control temperature at 122～125 ℃ of reaction 15～20min; Continue to add the sal volatile of liquid glucose quality 1～1.5%, control temperature at 120～122 ℃ of reaction 10～15min; Then control temperature at 115～120 ℃ of reaction 20～30min, finish reaction, obtain the caramel colorant of low 4-methylimidazole content.
2. preparation technology according to claim 1, is characterized in that: step (1), by after molasses dilution, be warming up to 105～110 ℃ and maintain after 40～60min, and be cooled to 60～80 ℃, carry out sedimentation.
3. preparation technology according to claim 2, is characterized in that: step (1), by molasses dilution, regulate behind pH to 1.5～2.8, and heat up.
4. preparation technology according to claim 1, is characterized in that: step (1), get after pellucid syrup governor weight degree to 60～65 ° Bx.
5. preparation technology according to claim 1, is characterized in that: step (2), liquid glucose is proceeded to reactor, and be warming up to after 115 ℃～120 ℃, add sal volatile.
6. preparation technology according to claim 1, is characterized in that: sal volatile is saturated aqueous solution.
7. preparation technology according to claim 1, is characterized in that: step (2), after finishing to react, is cooled to below 50 ℃.
8. preparation technology according to claim 1, is characterized in that: step (1), by molasses and water by weight 1:0.2～0.25 dilution.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105062132A (en) * | 2015-09-10 | 2015-11-18 | 千禾味业食品股份有限公司 | Ammonium sulfite method-based caramel colour production process |
| WO2015195969A3 (en) * | 2014-06-18 | 2016-03-31 | The Coca-Cola Company | Method for reducing low molecular weight species in caramel |
| CN106189350A (en) * | 2016-07-15 | 2016-12-07 | 千禾味业食品股份有限公司 | A kind of reduce the production technology of 4 Methylimidazole. content in ammonia caramel color |
| CN107474585A (en) * | 2017-08-28 | 2017-12-15 | 广西顶俏食品有限公司 | A kind of preparation method of solid caramel pigment |
| CN115644415A (en) * | 2022-10-25 | 2023-01-31 | 佛山市海天(高明)调味食品有限公司 | Dark soy sauce and preparation method thereof |
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| CN102993767A (en) * | 2012-12-13 | 2013-03-27 | 广州双桥股份有限公司 | Process for continuous preparation of caramel pigment by ammonium sulfite method |
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| CN102020870A (en) * | 2010-12-27 | 2011-04-20 | 岳阳湘渝焦糖实业有限公司 | Production technology of bright caramel |
| CN102993767A (en) * | 2012-12-13 | 2013-03-27 | 广州双桥股份有限公司 | Process for continuous preparation of caramel pigment by ammonium sulfite method |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015195969A3 (en) * | 2014-06-18 | 2016-03-31 | The Coca-Cola Company | Method for reducing low molecular weight species in caramel |
| CN106455644A (en) * | 2014-06-18 | 2017-02-22 | 可口可乐公司 | Method for reducing low molecular weight species in caramel |
| JP2017518057A (en) * | 2014-06-18 | 2017-07-06 | ザ コカ・コーラ カンパニーＴｈｅ Ｃｏｃａ‐Ｃｏｌａ Ｃｏｍｐａｎｙ | Method for reducing low molecular weight species in caramel |
| EP3157352A4 (en) * | 2014-06-18 | 2018-05-30 | The Coca-Cola Company | Method for reducing low molecular weight species in caramel |
| US10575535B2 (en) | 2014-06-18 | 2020-03-03 | The Coca-Cola Company | Method for reducing low molecular weight species in caramel |
| US11980206B2 (en) | 2014-06-18 | 2024-05-14 | The Coca-Cola Company | Method for reducing low molecular weight species in caramel |
| CN105062132A (en) * | 2015-09-10 | 2015-11-18 | 千禾味业食品股份有限公司 | Ammonium sulfite method-based caramel colour production process |
| CN106189350A (en) * | 2016-07-15 | 2016-12-07 | 千禾味业食品股份有限公司 | A kind of reduce the production technology of 4 Methylimidazole. content in ammonia caramel color |
| CN106189350B (en) * | 2016-07-15 | 2017-06-23 | 千禾味业食品股份有限公司 | A kind of production technology for reducing by 4 methylimidazole contents in ammonia caramel color |
| CN107474585A (en) * | 2017-08-28 | 2017-12-15 | 广西顶俏食品有限公司 | A kind of preparation method of solid caramel pigment |
| CN115644415A (en) * | 2022-10-25 | 2023-01-31 | 佛山市海天(高明)调味食品有限公司 | Dark soy sauce and preparation method thereof |
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Inventor after: Zhao Biqiu Inventor after: Lu Zhenting Inventor after: Li Yuhong Inventor after: Chang Guowei Inventor after: Tan Wenxing Inventor after: Deng Guanghua Inventor after: Liang Dafeng Inventor after: Nong Lizhong Inventor after: Huang Yunan Inventor after: Cai Biyun Inventor after: Zhong Yingping Inventor after: Yi Ximiao Inventor before: Zhao Biqiu Inventor before: Lu Zhenting Inventor before: Li Yuhong Inventor before: Chang Guowei Inventor before: Tan Wenxing Inventor before: Deng Guanghua Inventor before: Liang Dafeng Inventor before: Nong Lizhong Inventor before: Huang Yunan Inventor before: Cai Biyun Inventor before: Zhong Yingping Inventor before: Yi Ximiao |
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Effective date of registration: 20171109 Address after: 510760, No. 362, Pioneer Road, Whampoa District, Guangdong, Guangzhou Co-patentee after: Guangdong Province Institute of Biological Engineering (Guangzhou Sugarcane Industry Research Institute) Patentee after: Guangzhou Hua Sugar Food Co., Ltd. Address before: 510760, Guangdong province Guangzhou economic and Technological Development Zone, East Zone, No. 372 Co-patentee before: Guangzhou Sugarcane Industry Research Institute Patentee before: Gaungzhou Huaqiao Sugar Factory |
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