阅读说明：本技术 一种不含嗜酸耐热菌的果葡糖浆的生产方法 (Production method of high fructose corn syrup without acidophilic thermophilic bacteria ) 是由 刘峰 李克文 高义国 薛雅莺 孟文文 赵吉春 于 2019-09-11 设计创作，主要内容包括：本发明涉及一种不含嗜酸耐热菌的果葡糖浆的生产方法,淀粉乳经高浓液化、糖化、异构、色谱、精制、膜过滤、除菌过滤、浓缩等一系列处理及对生产过程各工序有序的清洁消毒措施,确保了最终生产出不含嗜酸耐热菌的果葡糖浆产品。本发明的优点在于：液化采用高浓液化有一定的抑菌作用和节能作用,为了保证源头料液的嗜酸耐热菌引入风险,对液化工序采用喷射液化温度125—148℃进行高温杀菌,另外在生产过程中对异构、色谱工序制定一定的消毒措施,预防生产过程中嗜酸耐热菌的滋生,尽量在生产过程中不留嗜酸耐热菌滋生死角。该工艺简便可行,利于进行工业化生产控制,提升果葡糖浆产品质量。(The invention relates to a method for producing high fructose corn syrup without acidophilic thermophilic bacteria, which ensures that high fructose corn syrup products without acidophilic thermophilic bacteria are finally produced by a series of treatments of high-concentration liquefaction, saccharification, isomerization, chromatography, refining, membrane filtration, sterilization filtration, concentration and the like and ordered cleaning and disinfection measures for each procedure in the production process. The invention has the advantages that: the liquefaction adopts high enriched liquefaction to have certain bacteriostatic action and energy-conserving effect, introduces the risk in order to guarantee the acidophilic heat-resisting fungus of source feed liquid, adopts injection liquefaction temperature 125-148 ℃ to carry out pasteurization to the liquefaction process, formulates certain disinfection measure to isomerism, chromatogram process in addition in process of production, prevents breeding of acidophilic heat-resisting fungus in process of production, does not leave acidophilic heat-resisting fungus as far as possible and breeds the dead angle in process of production. The process is simple, convenient and feasible, is beneficial to industrial production control, and improves the quality of the high fructose corn syrup product.)

1. A method for preparing high fructose corn syrup without thermophilic bacteria comprises the following steps:

the method comprises the following steps of carrying out size mixing, liquefaction, saccharification, slag removal, primary decolorization and filtration, primary ion exchange, primary concentration, isomerization, secondary decolorization and filtration, secondary ion exchange, membrane filtration, sterilization and filtration and secondary concentration on raw starch;

the liquefaction process adopts more than two times of jet liquefaction, and the last liquefaction temperature is 125-148 ℃;

the membrane used in the membrane filtration process is a 0.1 micron membrane, and the sterilizing filter used in the sterilizing filtration process is a sterilizing filter with the pore diameter less than or equal to 0.45 micron.

2. The method for preparing high fructose corn syrup without thermophilic bacteria according to claim 1, wherein the raw starch is corn starch, wheat starch, tapioca starch, rice starch, potato starch or sweet potato starch.

3. The method for preparing high fructose corn syrup without thermophilic bacteria as claimed in claim 1, wherein in the step of mixing, the starch is mixed into starch milk with a concentration of 20-23 baume degrees (° B), the pH is adjusted to 5.9, the high temperature resistant alpha-amylase is added, and the mixture is stirred uniformly.

4. The method for preparing high fructose corn syrup without thermophilic bacteria as claimed in claim 1, wherein the temperature of the first injection liquefaction is 105-.

5. The method according to claim 1, wherein the preparation process of F55 and high fructose corn syrup with fructose content > 55% further comprises the steps of secondary concentration, chromatographic separation, tertiary decolorization and filtration, tertiary ion exchange, sterilization and filtration, and tertiary concentration and mixing.

6. The method for preparing high fructose corn syrup without thermophilic bacteria according to claim 1, wherein the saccharification tank, the storage tank, the finished product tank and the pipeline involved in the whole preparation process are cleaned by CIP, the cleaning agent is sodium hydroxide solution with mass concentration of 1.5-3.5%, and the temperature is 60-90 ℃; the water used for preparing the cleaning agent is purified water, the water quality reaches the standard of drinking water, and the temperature is more than 85 ℃.

7. The method for preparing high fructose corn syrup without thermophilic acidophilic bacteria as claimed in claim 6, wherein the CIP cleaning cycle is performed after each emptying of the finished product tank, CIP cleaning and disinfection are performed only by purified water with temperature > 85 ℃ in the finished product tank, and the time is counted by the temperature of the outlet water of the cleaning tank being greater than or equal to 85 ℃, and the disinfection time is greater than or equal to 20 minutes.

8. The method for preparing high fructose corn syrup without thermophilic bacteria as claimed in claim 6, wherein the cleaning and disinfection of all sugar-making equipment pipelines, storage tanks and empty finished product tanks with CIP lye is carried out before and after each start-up and shut-down, and then the disinfection is carried out with purified water at a temperature of more than 85 ℃ for a disinfection time of more than or equal to 30 minutes.

9. The method for producing high fructose corn syrup containing no thermophilic acidophilic bacteria according to claim 6, wherein the isomerization step in which CIP sterilization is impossible is carried out by increasing the amount of the isomerase-protecting agent added;

preferably, the isomerase enzyme is protectedThe protective agent is sodium sulfite, sodium pyrosulfite or sodium thiosulfate, the addition amount of the isomerase protective agent is more than 1.1 times of the original addition amount, and the original addition amount is controlled to be [ SO ]₃]^2-At 110 ppm;

preferably, in the chromatographic separation process incapable of being sterilized by CIP, the chromatographic resin is sterilized at a high temperature at a temperature which can be satisfied by the resin; further preferably, the sterilization is carried out at a temperature of > 85 ℃ or at a maximum temperature suitable for the resin, and the sterilization operation time is not less than 3 hours.

10. The method for producing high fructose corn syrup without thermophilic bacteria according to claim 1, wherein the membrane used in the membrane filtration step is a 0.1 μm membrane;

the membrane is preferably an organic membrane, a ceramic membrane or a membrane made of other materials, and the degerming filter used after the membrane is the degerming filter with the pore diameter less than or equal to 0.45 micron.

The technical field is as follows:

the invention relates to a production method of high fructose corn syrup without thermophilic bacteria, belongs to the technical field of high fructose corn syrup preparation, and particularly relates to a production method of high fructose corn syrup prepared by starch milk through a series of processes, a method for cleaning and disinfecting each process in the production process, and finally high fructose corn syrup without thermophilic bacteria prepared by concentrating feed liquid after membrane filtration and sterilization filtration.

Background art:

high fructose corn syrup is starch syrup prepared by hydrolyzing and isomerizing vegetable starch, and is an important sweetener. Because its composition is mainly fructose and glucose; therefore, it is called "fructose-glucose syrup". According to the content of fructose, the high fructose corn syrup is divided into three types: the first type of high fructose corn syrup (F42 type) contains 42 percent of fructose; the second type of high fructose corn syrup (F55 type) contains 55% of fructose; the third type of high fructose corn syrup (type F90) contains 90% fructose. The sweetness of the high fructose corn syrup is directly correlated with the fructose content (see Iriseau et Perissima. soft drink processing technology and formula: chemical industry Press, 2006: 5). The high fructose corn syrup is applied to various food fields as a substitute of white granulated sugar, and the high fructose corn syrup product is favored by the industries of fruit juice and fruit drink by the good application characteristic and the mouthfeel similar to natural fruit flavor.

Thermotolerant acidophilic bacteria were first discovered in 1984 and were isolated from relatively rotten apple juice by Cerny et al, under the research nomenclature: bacillus acidoterrestris (Alicyclobacillus acidoter-retricis). The product is commonly called acidophilic thermophilic bacteria because of its acid-resistant and heat-resistant characteristics (see: research progress of detection technology and control method of acidophilic thermophilic bacteria, Liu Ying Sha, etc., proceedings of Yangling institute of occupational technology, vol.17, No. 1, 2018, 3 months). The acidophilic thermophilic bacterium is used as a bacterium which is extremely painful in the fruit juice industry, and the harm of the acidophilic thermophilic bacterium to the fruit juice industry is as follows: the bacterium does not generate gas and change the pH value of the fruit juice; can make the product turbid and generate white precipitate after packaging; can produce peculiar smell and make people dislike smell like smoke and herbal medicine; the bacteria do not produce toxic substances harmful to human. The amount of thermophilic bacteria which deteriorate the product. It is found in the united states: 76 spores in 236mL of apple juice can make it deteriorate within 24 h. It was found in australia that: the juice can deteriorate within 24 hours because each milliliter of juice contains 240-790 thalli; the australian standard holds that: more than 100 spores can cause the product to be off-flavored. High fructose corn syrup is used as an important raw material in the fruit juice and fruit drink industries, and strict control on acidophilic thermophilic bacteria is required.

At present, the preparation process of the high fructose corn syrup mainly comprises the following steps: starch-size mixing-saccharification-neutralization-decoloration-filtration-resin treatment-evaporation-isomerization-decoloration-resin treatment-evaporation-finished product. Meanwhile, Chinese patent document CN109609569A discloses a preparation method of sweet potato high fructose corn syrup, which comprises a compound enzyme method sweet potato glucose syrup preparation process, a process of isomerizing glucose isomerase into fructose, a syrup decoloring process, a syrup eluting and concentrating process and the like. Chinese patent document CN109402191A discloses a preparation method of rice F55 high fructose corn syrup. Chinese patent document CN109182422A discloses a production method of high fructose corn syrup, which comprises the steps of (1) washing and soaking, (2) grinding and mixing, (3) liquefying and spraying, (4) deproteinizing, (5) saccharifying, (6) decoloring and fine filtering, (7) primary ion exchange, (8) fixing glucose, (9) secondary ion exchange, and (10) carrying out secondary decoloring and fine filtering-sterilization, filtering-concentration-filling on the mixture obtained in the step (9). However, the preparation process of the high fructose corn syrup does not involve the control of the thermophilic bacteria.

At present, in the preparation process of the high fructose corn syrup, strict control is carried out on thermophilic acidophilic bacteria, so that the final high fructose corn syrup product does not contain thermophilic acidophilic bacteria, and no report is found. Accordingly, the present invention is set forth.

The invention content is as follows:

aiming at the defects of the prior art, the invention provides the production method of the high fructose corn syrup which is simple in steps and suitable for industrial popularization and does not contain acidophilic thermophilic bacteria.

The technical scheme of the invention is as follows:

a method for preparing high fructose corn syrup without thermophilic bacteria comprises the following steps:

the method comprises the following steps of carrying out size mixing, liquefaction, saccharification, slag removal, primary decolorization and filtration, primary ion exchange, primary concentration, isomerization, secondary decolorization and filtration, secondary ion exchange, membrane filtration, sterilization and filtration and secondary concentration on raw starch;

the liquefaction process adopts more than two times of jet liquefaction, and the last liquefaction temperature is 125-148 ℃;

the membrane used in the membrane filtration process is a 0.1 micron membrane, and the sterilizing filter used in the sterilizing filtration process is a sterilizing filter with the pore diameter less than or equal to 0.45 micron.

According to the present invention, preferably, the raw starch is corn starch, wheat starch, tapioca starch, rice starch, potato starch or sweet potato starch;

preferably, in the size mixing step, the starch is mixed into starch milk with the concentration of 20-23 baume degrees (Bee), the pH value is adjusted to 5.9, the high-temperature resistant alpha-amylase is added, and the mixture is uniformly stirred.

According to the invention, preferably, the primary injection liquefaction temperature in the liquefaction process is 105-115 ℃, the flash evaporation cooling is performed, the heat preservation is performed in the laminar flow tank, and then the next injection liquefaction is performed. Through two times of injection liquefaction or multiple times of injection liquefaction, the final liquefied liquid does not contain acidophilic thermophilic bacteria.

According to the invention, the preparation process can be applied to the preparation of F42 high fructose corn syrup. For the preparation process of F55 and high fructose corn syrup with fructose content more than 55%, the preparation process further comprises the working procedures of secondary concentration, chromatographic separation, tertiary decolorization and filtration, tertiary ion exchange after the secondary ion exchange and before membrane filtration, and the working procedures of tertiary concentration and mixing after sterilization and filtration.

According to the invention, preferably, the saccharification tank, the storage tank, the finished product tank and the pipeline involved in the whole preparation process are cleaned by CIP, and the cleaning agent is a sodium hydroxide solution with the mass concentration of 1.5-3.5% and the temperature is 60-90 ℃; the water used for preparing the cleaning agent is purified water, the water quality reaches the standard of drinking water, and the temperature is more than 85 ℃. The cleaning period is once per week or established according to production conditions. After each evacuation.

According to the invention, preferably, for the finished product tank, the CIP cleaning cycle is performed after each emptying, the CIP cleaning and disinfection of the finished product tank are only performed by using purified water with the temperature of more than 85 ℃, the time is counted by the temperature of the effluent of the cleaning tank being more than or equal to 85 ℃, and the disinfection time is more than or equal to 20 minutes.

According to the invention, preferably, before starting and after stopping, all sugar-making equipment pipelines, storage tanks and empty finished product tanks are cleaned and disinfected by CIP lye, and then disinfected by purified water with the temperature of more than 85 ℃, and the disinfection time is more than or equal to 30 minutes.

According to the present invention, it is preferable that the sterilization work of the isomerase is performed by increasing the amount of the isomerase protecting agent to be added to the isomerization step in which the CIP sterilization cannot be performed;

preferably, the isomerase protective agent is sodium sulfite, sodium pyrosulfite or sodium thiosulfate, the addition amount of the isomerase protective agent is more than 1.1 times of the original addition amount, and the original addition amount is controlled to be [ SO ]₃]^2-At 110ppm, the duty cycle is weekly or sporadically.

According to the present invention, it is preferable that, in the chromatographic separation step in which CIP sterilization cannot be performed, the chromatographic resin is subjected to a high-temperature sterilization operation at a temperature that can be satisfied by the resin; further preferably, the sterilization is carried out at a temperature of > 85 ℃ or at a maximum temperature suitable for the resin, and the sterilization operation time is not less than 3 hours. The period of the sterilization operation is set according to the production condition.

According to the present invention, the membrane used in the membrane filtration step is preferably a 0.1 micron membrane, more preferably an organic membrane, a ceramic membrane or a membrane made of other materials, and the sterilizing filter used after the membrane filtration step is a sterilizing filter having a pore size of 0.45 micron or less. The membrane filtration is arranged in front of the sterilizing filter, so that the membrane filtration has the function of effectively intercepting impurity particles and has a certain effect of intercepting partial dead bacteria and live bacteria. Because the membrane core replacement period is longer, about 3 years of organic membranes, the ceramic membrane is more as long as 5-10 years, in order to prevent the membrane from polluting the product quality of the finished high fructose syrup product and better intercept and remove microbial thalli, the high fructose syrup product without acidophilic heat-resistant bacteria is ensured to be produced, and after the membrane filtration, a sterilizing filter with the aperture not more than 0.45 micron is added for effective interception, so that the product quality is ensured and improved.

The production process of the main product of the invention mainly comprises the following procedures:

1. f42 high fructose corn syrup production process:

starch (starch milk) → size mixing → primary liquefaction → secondary liquefaction → saccharification → deslagging → primary decolorization and filtration → primary ion exchange → primary concentration → isomerism → secondary decolorization and filtration → secondary ion exchange → membrane filtration → sterilization and filtration → secondary concentration → finished product storage → filling → delivery.

2. F55 and a high fructose corn syrup production process with fructose content more than 55 percent:

starch (starch milk) → size mixing → first liquefaction → second liquefaction → saccharification → deslagging → first decolorization and filtration → first ion exchange → first concentration → isomerism → second decolorization and filtration → second ion exchange → second concentration → chromatographic separation → third decolorization and filtration → third ion exchange and membrane filtration → sterilization and filtration → third concentration → mixing → finished product storage → filling → delivery.

The present invention has been described in detail in accordance with the prior art.

The starch is subjected to a series of treatments such as size mixing, liquefaction, saccharification, isomerization, chromatographic separation, membrane filtration, sterilization filtration, concentration and the like, and orderly cleaning and disinfection measures for all working procedures in the production process, so that the final production of the high fructose corn syrup product without acidophilic thermophilic bacteria is ensured.

The invention has the advantages that:

1. the liquefaction adopts high concentration liquefaction to have certain bacteriostatic action and energy-conserving effect, and the liquefaction process adopts jet liquefaction temperature 125-148 ℃ to carry out high temperature sterilization, has guaranteed not to introduce acidophilic thermophilic bacteria in the source feed liquid, has stopped acidophilic thermophilic bacteria's introduction risk from the source.

2. In the production process, disinfection measures are made for isomerism and chromatographic procedures, the breeding of acidophilic thermophilic bacteria in the production process is prevented, and no acidophilic thermophilic bacteria breeding dead angle is left in the production process as much as possible.

3. The invention puts the membrane filtration in front of the sterilizing filter, which can effectively intercept the impurity particles and can intercept part of dead bacteria and live bacteria. Because the membrane core replacement period is longer, the organic membrane is about 3 years, the ceramic membrane is as long as 5-10 years, in order to prevent the membrane from polluting the product quality of the finished high fructose syrup product and better intercept and remove microbial thalli, the high fructose syrup product without acidophilic heat-resistant bacteria is ensured to be produced, and therefore, a sterilizing filter with the pore diameter less than or equal to 0.45 micrometer is added after the membrane filtration for effective interception, and the product quality is ensured and improved.

4. The method is simple, convenient and feasible, is beneficial to industrial production control, improves the quality of the high fructose corn syrup product, and prepares the high fructose corn syrup product without acidophilic thermophilic bacteria.

The specific implementation mode is as follows:

the present invention is further illustrated by, but is not limited to, the following specific examples.