CN103772524A - Preparation method of water soluble soybean polysaccharide for improving capacity of stabilizing lactoprotein particles - Google Patents
Preparation method of water soluble soybean polysaccharide for improving capacity of stabilizing lactoprotein particles Download PDFInfo
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Abstract
The invention discloses a preparation method of water soluble soybean polysaccharide for improving capacity of stabilizing lactoprotein particles, belonging to the field of processing of subsidiary agricultural products. The method is more specifically a method of combining an alkaline agent to chemically modify to remove methoxyl groups to improve the capacity of stabilizing lactoprotein particles of water soluble soybean polysaccharide. The method comprises the following steps: first, preparing bean dregs into a suspension; after using the alkaline agent to chemically modify to remove methoxyl groups, further extracting by hot water through an acid process; and after removing salt, alcohol soluble small molecular matters and water by ethanol for the water soluble soybean polysaccharide liquor obtained by extraction, drying to obtain the water soluble soybean polysaccharide with strong capacity of stabilizing lactoprotein particles. The preparation method disclosed by the invention not only effectively improves the by-product utilization ratio of a bean processing plant so as to avoid wasting of resources, but also the water soluble soybean polysaccharide obtained has very good capacity of stabilizing lactoprotein particles.
Description
Technical field
The invention discloses a kind of preparation method who improves the water soluble soybean polysaccharide of stablizing milk-protein particle ability, the method that more particularly removes methoxyl group and improve water soluble soybean polysaccharide and stablize milk-protein particle ability in conjunction with the processing of alkaline agent chemical modification, belongs to agricultural byproducts processing technical field.
Background technology
Water soluble soybean polysaccharide is from pulse family soybean sporophore and leaf, to extract the water-soluble polysaccharides material obtaining.In the time producing soybean protein isolate, bean curd stick or bean curd, have the generation of a large amount of by product bean dregs, wherein contain about 55% water soluble soybean polysaccharide.Producing food fibre, utilize by product bean dregs can produce water soluble soybean polysaccharide.Due to physico-chemical properties such as the low viscosity of water soluble soybean polysaccharide, biocidal property, film-forming propertiess, water soluble soybean polysaccharide not only has physiological function of diet fiber characteristic, can also well be applied to and in food, improve food system functional performance; Can be used as additive and be added to the product that obtains clean taste in yogurt drink.Therefore, water soluble soybean polysaccharide has a extensive future in food service industry.
Water soluble soybean polysaccharide is to be mainly applied in yogurt drink as stablizer.Water soluble soybean polysaccharide is having relevant commercially produced product on the market at present, but the ability of its stable milk-protein particle of the water soluble soybean polysaccharide of these commercially produced products is undesirable; In the time being applied in yogurt drink, although can obtain salubrious good to eat product, can not serve as stablizer and well stablize milk-protein particle, in long-term put procedure, have the generation of suspended substance, throw out or demixing phenomenon; In emulsion system, the water soluble soybean polysaccharide of commercially produced product can not form good O/W emulsion system as stablizer.In the time producing water soluble soybean polysaccharide, industrial yield and the purity generally paid attention to, is applied to the functional effect in food and ignored water soluble soybean polysaccharide.
After methoxyl group is the hydrogen atom removing in methanol molecules on hydroxyl, remaining univalent perssad, structural formula is: CH
3o
-, be the simplest a kind of alkoxyl group.Water soluble soybean polysaccharide is made up of semi-lactosi, pectinose, wood sugar, seminose, glucose, rhamnosyl and uronic acid; Wherein on uronic acid, have many methoxy group, these methoxy group have remarkably influenced to the functional performance of water soluble soybean polysaccharide.The water soluble soybean polysaccharide of different methoxy contents is applied to and in food system, shows different characteristics.Research shows, the methoxy content in water soluble soybean polysaccharide is higher, and its ability of stablizing milk-protein particle in yogurt drink is lower, otherwise if its methoxy content is lower, the ability of stablizing so milk-protein particle in yogurt drink is stronger.Therefore in extraction water soluble soybean polysaccharide, increase methoxyl group removing process, its water soluble soybean polysaccharide of producing is stablized the ability of milk-protein particle and will be improved.
The present invention has well solved water soluble soybean polysaccharide and has been applied to the problems such as suspended substance, throw out or layering that the medium-term and long-term placement of yogurt drink produces, has proposed the processing of a kind of alkaline agent chemical modification and has removed methoxyl group and combine to extract with acid system hot water the method for stablizing the water soluble soybean polysaccharide that milk-protein particle ability is strong.First bean dregs suspension is carried out to the processing of alkaline agent chemical modification and remove methoxyl group, further adopt acid system hot water extraction to obtain water soluble soybean polysaccharide solution, remove salt, the molten small-molecule substance of alcohol and water post-drying through ethanol and obtain stablizing the strong water soluble soybean polysaccharide of milk-protein particle ability.The present invention's cost of material used is cheap, reagent and method safety, and economy, practical, suitability for industrialized production is simple and easy to control, and product has the ability of stablizing milk-protein particle preferably.
Summary of the invention
The invention solves water soluble soybean polysaccharide and stablize the problem of milk-protein particle ability, eliminate it and be applied to the phenomenons such as suspended substance, throw out or layering that the medium-term and long-term placement of yogurt drink occurs, proposed a kind ofly to process demethoxylation based on alkaline agent chemical modification and combine to extract with acid system hot water the method for stablizing the water soluble soybean polysaccharide that milk-protein particle ability is strong.Bean dregs suspension is carried out to the processing of alkaline agent chemical modification and remove after methoxyl group, the further acid system hot water extraction of wet bean dregs obtaining obtains water soluble soybean polysaccharide solution; Add ethanol to remove salt, the molten small molecules of alcohol and the acquisition of water post-drying and stablize the strong water soluble soybean polysaccharide of milk-protein particle ability.The measurement index of " stablizing milk-protein particle ability " in the present invention is centrifugation rate.
Technical scheme provided by the invention, a kind of preparation method who improves the water soluble soybean polysaccharide of stablizing milk-protein particle ability: use alkaline agent to remove after methoxyl group to the bean dregs suspension preparing, adopt acidizer to carry out acid system hot water extraction, obtain water soluble soybean polysaccharide solution, after ethanol removes salt, the molten small-molecule substance of alcohol and water, dry and obtain stablizing the good water soluble soybean polysaccharide of milk-protein particle ability;
Concrete steps are as follows:
(1) alkaline agent processing: get dry bean dregs, by dry bean dregs: water solid-liquid ratio is that 1:10-40 dissolves, and adds alkaline agent to remove methoxyl group, control pH is 9.0-13.0, regulate temperature 50-90 ℃, reaction times 30-180min, the after completion of the reaction centrifugal wet bean dregs of thing that are precipitated under 3500rpm;
(2) acidizer processing: the wet bean dregs of preparing by step (1): water weight ratio is that 1:1.0-4.0 dissolves, carry out acid system hot-water cure by acidizer, adding acidizer control pH is 3.0-5.0, temperature is 110-140 ℃, reaction times is 60-180min, centrifugal 30min under 5000g, gets supernatant liquor after completion of the reaction;
(3) Ethanol Treatment: the supernatant liquor that step (2) is obtained and ethanol are by weight mixing for 1:1-5, regulating pH value with acidizer or alkaline agent is 7.0, suction filtration is precipitated, and obtains product and improves and stablize the water soluble soybean polysaccharide of milk-protein particle ability being deposited in 50 ℃ of oven for drying.
The described alkaline agent treatment condition of step (1) are: dry bean dregs and aqueous solution ratio are 1:20-30, add the processing of alkaline agent chemical modification to remove methoxyl group, and control pH is 11.0-12.0, and adjusting temperature is 70-80 ℃, reaction times 90-120min.
The described acidizer treatment condition of step (2) are: wet bean dregs and water weight ratio are that 1:1.5-2.0 dissolves, and carry out acid system hot-water cure by acidizer, and pH is 4.0-4.5, and temperature is 120-125 ℃, and the reaction times is 120-150min.
The described alkaline agent of step (1) is the one in sodium hydroxide, potassium hydroxide or calcium hydroxide.The described alkaline agent of step (1) is sodium hydroxide.
The described acidizer of step (2) is citric acid, hydrochloric acid or acetic acid.The described acidizer of step (2) is hydrochloric acid.
Show after deliberation, the methoxy group content in water soluble soybean polysaccharide has significant impact on water soluble soybean polysaccharide in the stabilizing power of yogurt drink.Therefore the present invention, from reducing the angle of methoxy group content, has proposed the processing of employing alkaline agent chemical modification and has removed methoxy group; Under alkaline condition, methoxy group above water soluble soybean polysaccharide gradually be converted into carboxylate group, successfully realize the chemical modification effect after alkaline purification, thereby reduced methoxy content, the functional performance that methoxy group shows is weakened; Along with the reduction gradually of the structural methoxy group of water soluble soybean polysaccharide, the ability of its stable milk-protein particle also becomes and becomes better and better.
In the inventive method, acid system hot water extraction is mainly the fibres sugars glycosidic bond degraded making in bean dregs, has formed the polysaccharose substance of molecular weight in 5000-500000 scope, improves the extraction yield of water soluble soybean polysaccharide; But can not reduce the methoxy group content above water soluble soybean polysaccharide, thereby restrict water soluble soybean polysaccharide and stablize the ability of milk-protein particle.
Beneficial effect of the present invention: the inventive method has proposed first to utilize the processing of simple, efficient, manageable alkaline agent chemical modification to remove methoxyl group and combined and be applied in the production of water soluble soybean polysaccharide with acid system hot water extraction.By the alkaline agent chemical modification processing of bean dregs suspension, reduce the methoxy content of polysaccharose substance in bean dregs solution, thereby the water soluble soybean polysaccharide methoxy group obtaining reduces, in Long-term Storage, there will not be the phenomenon of suspended substance, throw out or layering with its stable yogurt drink; The present invention utilizes the processing of alkaline agent chemical modification to can be good at removing the methoxy group on water soluble soybean polysaccharide, and cost is lower, and suitability for industrialized production is easy to realize.
Accompanying drawing explanation
Fig. 1 is the required reagent of the measuring method of methoxy content and mensuration schema in Application Example.
Embodiment
Embodiment 1
Getting dry bean dregs 10g, dissolve by solid-liquid ratio 1:25, is 12 by controlling pH, 80 ℃ of temperature, and reaction times 90min carries out the processing of alkaline agent sodium hydroxide chemical modification and removes methoxyl group, then the centrifugal thing that is precipitated under 3500rpm.Throw out and water are pressed to solid-liquid ratio 1:1.5 dissolving, are 4.0 by controlling pH, 120 ℃ of temperature, and reaction times 150min carries out hydrochloric acid acid system hot-water cure, and then centrifugal 30min under 5000g, gets supernatant liquor.Supernatant liquor is mixed in 1 ︰ 3 ratios with ethanol, and use high-speed shearing machine is adjusted to 7.0 by pH with hydrochloric acid after shearing evenly, with Büchner funnel and vacuum pump, it is carried out to suction filtration and is precipitated.Obtain water soluble soybean polysaccharide 50 ℃ of oven for drying.Measure the ability of milk-protein particle in its methoxy content and stable acidic milky-drinks, in table 3.
Embodiment 2
Getting dry bean dregs 10g, dissolve by solid-liquid ratio 1:20, is 13 by controlling pH, temperature 70 C, and reaction times 120min carries out the processing of alkaline agent potassium hydroxide chemical modification and removes methoxyl group, then the centrifugal thing that is precipitated under 3500rpm.Throw out and water are pressed to solid-liquid ratio 1:2 dissolving, are 3.5 by controlling pH, 115 ℃ of temperature, and reaction times 60min carries out citric acid acid system hot-water cure, and then centrifugal 30min under 5000g, gets supernatant liquor.Supernatant liquor is mixed in 1 ︰ 3 ratios with ethanol, and use high-speed shearing machine is adjusted to 7.0 by pH with hydrochloric acid after shearing evenly, with Büchner funnel and vacuum pump, it is carried out to suction filtration and is precipitated.Obtain water soluble soybean polysaccharide 50 ℃ of oven for drying.Measure the ability of milk-protein particle in its methoxy content and stable acidic milky-drinks, in table 3.
Embodiment 3
Getting dry bean dregs 10g, dissolve by solid-liquid ratio 1:25, is 11 by controlling pH, 80 ℃ of temperature, and reaction times 90min carries out the processing of alkaline agent calcium hydroxide chemical modification and removes methoxyl group, then the centrifugal thing that is precipitated under 3500rpm.Throw out and water are pressed to solid-liquid ratio 1:2 dissolving, are 4.5 by controlling pH, 130 ℃ of temperature, and reaction times 60min carries out acetic acid acid system hot-water cure, and then centrifugal 30min under 5000g, gets supernatant liquor.Supernatant liquor is mixed in 1 ︰ 3 ratios with ethanol, and use high-speed shearing machine is adjusted to 7.0 by pH with hydrochloric acid after shearing evenly, with Büchner funnel and vacuum pump, it is carried out to suction filtration and is precipitated.Obtain water soluble soybean polysaccharide 50 ℃ of oven for drying.Measure the ability of milk-protein particle in its methoxy content and stable acidic milky-drinks, in table 3.
Embodiment 4
Getting dry bean dregs 10g, dissolve by solid-liquid ratio 1:30, is 12 by controlling pH, temperature 60 C, and reaction times 120min carries out the processing of alkaline agent sodium hydroxide chemical modification and removes methoxyl group, then the centrifugal thing that is precipitated under 3500rpm.Throw out and water are pressed to solid-liquid ratio 1:3 dissolving, be 5.0 by controlling pH, 135 ℃ of temperature, reaction times 120min carries out hydrochloric acid acid system hot-water cure, then centrifugal 30min under 5000g, gets supernatant liquor, and supernatant liquor is mixed in 1 ︰ 3 ratios with ethanol, after using high-speed shearing machine to shear evenly, pH is adjusted to 7.0 with hydrochloric acid, with Büchner funnel and vacuum pump, it is carried out to suction filtration and be precipitated.Obtain water soluble soybean polysaccharide 50 ℃ of oven for drying.Measure the ability of milk-protein particle in its methoxy content and stable acidic milky-drinks, in table 3.
Embodiment 5
Getting dry bean dregs 10g, dissolve by solid-liquid ratio 1:25, is 11 by controlling pH, temperature 70 C, and reaction times 90min carries out the processing of alkaline agent potassium hydroxide chemical modification and removes methoxyl group, then the centrifugal thing that is precipitated under 3500rpm.Throw out and water are pressed to solid-liquid ratio 1:2.5 dissolving, are 4.5 by controlling pH, 120 ℃ of temperature, and reaction times 150min carries out citric acid acid system hot-water cure, and then centrifugal 30min under 5000g, gets supernatant liquor.Supernatant liquor is mixed in 1 ︰ 3 ratios with ethanol, and use high-speed shearing machine is adjusted to 7.0 by pH with hydrochloric acid after shearing evenly, with Büchner funnel and vacuum pump, it is carried out to suction filtration and is precipitated.Obtain water soluble soybean polysaccharide 50 ℃ of oven for drying.Measure the ability of milk-protein particle in its methoxy content and stable acidic milky-drinks, in table 3.
Embodiment 6
Getting dry bean dregs 10g, dissolve by solid-liquid ratio 1:20, is 12 by controlling pH, temperature 50 C, and reaction times 150min carries out the processing of alkaline agent calcium hydroxide chemical modification and removes methoxyl group, then the centrifugal thing that is precipitated under 3500rpm.Throw out and water are pressed to solid-liquid ratio 1:2.5 dissolving, are 4.5 by controlling pH, 130 ℃ of temperature, and reaction times 120min carries out acetic acid acid system hot-water cure, and then centrifugal 30min under 5000g, gets supernatant liquor.Supernatant liquor is mixed in 1 ︰ 3 ratios with ethanol, and use high-speed shearing machine is adjusted to 7.0 by pH with hydrochloric acid after shearing evenly, with Büchner funnel and vacuum pump, it is carried out to suction filtration and is precipitated.Obtain water soluble soybean polysaccharide 50 ℃ of oven for drying.Measure the ability of milk-protein particle in its methoxy content and stable acidic milky-drinks, in table 3.
Embodiment 7
Getting dry bean dregs 10g, dissolve by solid-liquid ratio 1:20, is 10 by controlling pH, 90 ℃ of temperature, and the processing of reaction times 60min alkaline agent sodium hydroxide chemical modification removes methoxyl group, the then centrifugal thing that is precipitated under 3500rpm.Throw out and water are pressed to solid-liquid ratio 1:1.5 dissolving, are 4.0 by controlling pH, 120 ℃ of temperature, and reaction times 120min carries out hydrochloric acid acid system hot-water cure, and then centrifugal 30min under 5000g, gets supernatant liquor.Supernatant liquor is mixed in 1 ︰ 3 ratios with ethanol, and use high-speed shearing machine is adjusted to 7.0 by pH with hydrochloric acid after shearing evenly, with Büchner funnel and vacuum pump, it is carried out to suction filtration and is precipitated.Obtain water soluble soybean polysaccharide 50 ℃ of oven for drying.Measure the ability of milk-protein particle in its methoxy content and stable acidic milky-drinks, in table 3.
Embodiment 8
Getting dry bean dregs 10g, dissolve by solid-liquid ratio 1:40, is 9 by controlling pH, 80 ℃ of temperature, and reaction times 60min carries out the processing of alkaline agent potassium hydroxide chemical modification and removes methoxyl group, then the centrifugal thing that is precipitated under 3500rpm.Throw out and water are pressed to solid-liquid ratio 1:1 dissolving, are 4.0 by controlling pH, 115 ℃ of temperature, and reaction times 180min carries out citric acid acid system hot-water cure, and then centrifugal 30min under 5000g, gets supernatant liquor.Supernatant liquor is mixed in 1 ︰ 3 ratios with ethanol, and use high-speed shearing machine is adjusted to 7.0 by pH with hydrochloric acid after shearing evenly, with Büchner funnel and vacuum pump, it is carried out to suction filtration and is precipitated.Obtain water soluble soybean polysaccharide 50 ℃ of oven for drying.Measure the ability of milk-protein particle in its methoxy content and stable acidic milky-drinks, in table 3.
Application Example 1
The measuring method of methoxy content: required reagent and mensuration flow process are as shown in Figure 1.
70% ethanol; Mix reagent: 5mL concentrated hydrochloric acid is that 70% ethanol is mixed to get mutually with 100mL mass concentration; Dehydrated alcohol; The standard solution of sodium hydroxide of 0.02mol/L and 0.5mol/L; The hydrochloric acid standard solution of 0.5mol/L; Phenolphthalein indicator: 1% phenolphthalein ethanolic soln.
Methoxy content calculation formula is:
V
1: the titre (mL) that sample solution is original
V
2: the titre (mL) of sample solution saponification
0.163: gamma value and methoxy content gain factor
Other conventional substances content assaying methods.105 ℃ of constant weight desiccating methods of moisture: GB5009.3-2010; Ash content: GB/T5009.4-2010 ashing method; Protein: GB/T 5009.5-2010 Kjeldahl determination; Polysaccharide: phenolsulfuric acid method.
The measuring method of centrifugation rate: water soluble soybean polysaccharide, skim-milk and water after drying are mixed with to yogurt drink, are warming up to 55 ℃, homogeneous under 40MPa; Wherein water soluble soybean polysaccharide content is 0.5%(W/W), milk protein content 1%(W/W), yogurt drink pH is 4.3.Yogurt drink after bus sterilization (85 ℃, 20min) is got to part centrifugal 20min under 3500rpm, take centrifugal front example weight and centrifuged deposit weight, calculate centrifugation rate; Calculate in this way firm processing, storage 7 days, storage 15 days and the centrifugation rate of storage after 30 days.
Centrifugation rate=centrifuged deposit weight/centrifugal front sample weight
Centrifugation rate is less, illustrates that the stable milk-protein particle ability of water soluble soybean polysaccharide is better.The free list 1 that is related to of centrifugation rate and stabilizing power illustrates.
Table 1
The composition (%) of the prepared water soluble soybean polysaccharide of embodiment 1-8 and on the market 2 kinds of (A and B) commercialization water soluble soybean polysaccharides of purchase is as shown in table 2.
Table 2
In the methoxy content (%) of the prepared water soluble soybean polysaccharide of embodiment 1-8 and on the market 2 kinds of (A and B) commercialization water soluble soybean polysaccharides of purchase and stable acidic milky-drinks thereof, the firm processing of milk-protein particle, storage 7 days, storage 15 days and centrifugation rate (%) situation of storage after 30 days are as shown in table 3.
Table 3
Can find out from experimental result shown in table 3, above-described embodiment 1-8 is that processing removes methoxyl group and is combined the water soluble soybean polysaccharide obtaining with acid system hot water extraction through alkaline agent chemical modification, it has different methoxy contents, and in its stable acidic milky-drinks, the effect of milk-protein will be significantly better than the commercialization water soluble soybean polysaccharide of buying on the market; Along with the reduction of methoxy content, the effect of its stable milk-protein particle is also progressively to strengthen; For the water soluble soybean polysaccharide of low-methoxyl content, its stable yogurt drink has presented good stability (embodiment 1 and 2) in storage after one month, all shows as " excellent ".And the water soluble soybean polysaccharide of high methoxyl content (commercialization A and B), yogurt drink stabilizing power after treatment show as " in ", storage two weeks after its stabilizing power show as " poor ".As can be seen here, the effect of the milk-protein particle in low, the stable acidic milky-drinks of water soluble soybean polysaccharide methoxy content prepared according to the methods of the invention is fine.
Present invention includes variation and advantage that person skilled in art can expect, take appending claims as assurance scope.
Claims (7)
1. one kind is improved the preparation method of the water soluble soybean polysaccharide of stablizing milk-protein particle ability, it is characterized in that: use alkaline agent to remove after methoxyl group to the bean dregs suspension preparing, adopt acidizer to carry out acid system hot water extraction, obtain water soluble soybean polysaccharide solution, after ethanol removes salt, the molten small-molecule substance of alcohol and water, dry and obtain stablizing the good water soluble soybean polysaccharide of milk-protein particle ability;
Concrete steps are as follows:
(1) alkaline agent processing: get dry bean dregs, by dry bean dregs: water solid-liquid ratio is that 1:10-40 dissolves, and adds alkaline agent to remove methoxyl group, control pH is 9.0-13.0, regulate temperature 50-90 ℃, reaction times 30-180min, the after completion of the reaction centrifugal wet bean dregs of thing that are precipitated under 3500rpm;
(2) acidizer processing: the wet bean dregs of preparing by step (1): water weight ratio is that 1:1.0-4.0 dissolves, carry out acid system hot-water cure by acidizer, adding acidizer control pH is 3.0-5.0, temperature is 110-140 ℃, reaction times is 60-180min, centrifugal 30min under 5000g, gets supernatant liquor after completion of the reaction;
(3) Ethanol Treatment: the supernatant liquor that step (2) is obtained and ethanol are by weight mixing for 1:1-5, regulating pH value with acidizer or alkaline agent is 7.0, suction filtration is precipitated, and obtains product and improves and stablize the water soluble soybean polysaccharide of milk-protein particle ability being deposited in 50 ℃ of oven for drying.
2. improve according to claim 1 the preparation method of the water soluble soybean polysaccharide of stablizing milk-protein particle ability, it is characterized in that: the described alkaline agent treatment condition of step (1) are: dry bean dregs and aqueous solution ratio are 1:20-30, add the processing of alkaline agent chemical modification to remove methoxyl group, control pH is 11.0-12.0, adjusting temperature is 70-80 ℃, reaction times 90-120min.
3. improve according to claim 1 the preparation method of the water soluble soybean polysaccharide of stablizing milk-protein particle ability, it is characterized in that: the described acidizer treatment condition of step (2) are: wet bean dregs and water weight ratio are that 1:1.5-2.0 dissolves, carry out acid system hot-water cure by acidizer, pH is 4.0-4.5, temperature is 120-125 ℃, and the reaction times is 120-150min.
4. the preparation method who improves according to claim 1 the water soluble soybean polysaccharide of stablizing milk-protein particle ability, is characterized in that: the described alkaline agent of step (1) is the one in sodium hydroxide, potassium hydroxide or calcium hydroxide.
5. the preparation method who improves according to claim 4 the water soluble soybean polysaccharide of stablizing milk-protein particle ability, is characterized in that: the described alkaline agent of step (1) is sodium hydroxide.
6. the preparation method who improves according to claim 1 the water soluble soybean polysaccharide of stablizing milk-protein particle ability, is characterized in that: the described acidizer of step (2) is citric acid, hydrochloric acid or acetic acid.
7. the preparation method who improves according to claim 6 the water soluble soybean polysaccharide of stablizing milk-protein particle ability, is characterized in that: the described acidizer of step (2) is hydrochloric acid.
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