Name | L-Leucine |
Synonyms | L-Leu Leucine H-Leu-OH L-Leucine 1-Leucine L(+)LEUCINE 4-methyl-norvalin 4-methyl-l-norvalin 2-amino-4-methyl-valericaci 2-amino-4-methylpentanoicacid 2-Amino-4-methylpentanoic acid (s)-2-amino-4-methylvalericacid (S)-2-Amino-4-methylpentanoic acid alpha-Amino-gamma-methylvaleric acid |
CAS | 61-90-5 200936-87-4 |
EINECS | 200-522-0 |
InChI | InChI=1/C6H13NO2/c1-4(2)3-5(7)6(8)9/h4-5H,3,7H2,1-2H3,(H,8,9)/t5-/m0/s1 |
Molecular Formula | C6H13NO2 |
Molar Mass | 131.17 |
Density | 1,293 g/cm3 |
Melting Point | >300 °C (lit.) |
Boling Point | 122-134 °C(Press: 2-3 Torr) |
Specific Rotation(α) | 15.4 º (c=4, 6N HCl) |
Flash Point | 145-148°C |
JECFA Number | 1423 |
Water Solubility | 22.4 g/L (20 C) |
Solubility | Very slightly dissolved in ethanol or ether, soluble in formic acid, dilute hydrochloric acid, alkaline hydroxide and carbonate solution. |
Vapor Presure | <1 hPa (20 °C) |
Appearance | White crystal |
Color | White to Off-white |
Maximum wavelength(λmax) | ['λ: 260 nm Amax: 0.05', , 'λ: 280 nm Amax: 0.05'] |
Merck | 14,5451 |
BRN | 1721722 |
pKa | 2.328(at 25℃) |
PH | 5.5-6.5 (20g/l, H2O, 20℃) |
Storage Condition | 2-8°C |
Stability | Stability Moisture and light sensitive. Incompatible with strong oxidising agents. |
Refractive Index | 1.4630 (estimate) |
MDL | MFCD00002617 |
Physical and Chemical Properties | melting point 286-288°C |
Use | Used as pharmaceutical raw materials and food additives |
Safety Description | 24/25 - Avoid contact with skin and eyes. |
WGK Germany | 3 |
RTECS | OH2850000 |
TSCA | Yes |
HS Code | 29224995 |
amino acid drugs. As amino acid infusion and comprehensive amino acid preparation. For the diagnosis and treatment of children with idiopathic hyperglycemia. And applicable to sugar metabolism disorders, accompanied by decreased bile secretion of liver disease, anemia, poisoning, muscular atrophy, polio sequelae, neuritis and psychosis. For oral administration, 20 ~ 30mL(3%), 3 times a day. For intravenous injection each 10 ~ 20mL (3%).
Blood meal [HCl (decomposition)]& rarr;[110 ℃, 24h] hydrolysate [acid removal] & rarr;[Vacuum distillation] acid removal [activated carbon (adsorption decolorization)]& rarr; Effluent [concentration] & rarr;[vacuum distillation] concentrate [precipitation] & rarr;[O-xylene -4-sulfonic acid] Precipitation [ammonia (free)]& rarr;[filtration] crude leucine [activated carbon (decoloration)]& rarr;[70 ℃, 1H] filtrate [concentrated crystallization] & rarr;[vacuum distillation] L-leucine crude [water (washing and drying) & rarr;L-leucine finished product
Hydrolysis and acid removal 500L of 6mol/L HCl solution was added to a 1T hydrolysis tank, and 100kg of animal blood powder was added, heated and incubated at 110-120 ° C. For 24h for reflux hydrolysis, and then concentrated under reduced pressure at 70-80 ° C. To a paste state. Then, 50L was added and concentrated to a paste form, which was repeated three times, cooled to room temperature, and the filtrate was collected by filtration to obtain a hydrolysate.
Adsorption and decolorization the hydrolysate was Diluted 1 times with water and then flowed into the granular activated carbon column (30cm × 180cm) at a flow rate of 0.5L/min until phenylalanine appeared in the effluent, the eluate was washed with deionized water at the same flow rate until the pH of the eluate was 4.0, and the effluent and the Wash were combined to obtain the effluent.
Concentration, precipitation and release after concentrating the effluent under reduced pressure to 1/3 of the original volume, 1/10 volume (V/V) of O-xylene-4-sulfonic acid is added under stirring, A precipitate of leucine sulfonate was produced, and the precipitate was taken by filtration, washed twice with 2 volumes of deionized water, and dried by Suction filtration to obtain the leucine sulfonate. Then, the mixture was stirred with 2 volumes of deionized water, and then 6mol/L ammonia water was added to neutralize to pH 6-8, and the mixture was stirred at 70-80 ° C. For 1H to free leucine from its sulfonate. The crystals were cooled, and the crystals were taken by filtration, then washed twice with 2 times the volume of deionized water, and dried by Suction filtration to obtain the crude leucine.
After refining, the crude leucine is heated and dissolved in 40 times the volume of deionized water, 0.5% activated carbon (5g/L) is added to keep the temperature at 70 ℃, stirred and decolorized for 1H, and the filtrate is filtered, after concentrating to 1/4 of the original volume, the crystals were cooled, taken by filtration, washed with a small amount of water, and dried at 70-80 ° C. To obtain a fine L-leucine product.
corn gluten [dehydrated and dried] & rarr; Corn gluten flour [ethanol extracted] & rarr; Corn gluten [hydrolyzed] & rarr; Hydrolysate [neutralized, decolorized] & rarr; decolorant [removal of tyrosine] & rarr; Filtrate [106-110 ℃, 20h; Concentration] & rarr; Concentrate [acid-soluble] & rarr; Precipitate [ammonolysis] & rarr; crude leucine [recrystallized] & rarr;L-leucine
Corn gluten powder preparation of corn gluten contains a lot of water, solid content accounts for about 20%-30%, need to be dehydrated, dry to produce corn gluten powder.
Corn gluten meal is prepared from corn gluten, extracted with 90%-95% ethanol solution, the extract is evaporated and concentrated to recover ethanol, and then precipitated with water to obtain corn gluten meal.
Hydrolysis of corn 10kg, industrial hydrochloric acid 27L, water 9L, into the hydrolysis tank, insulation 106-110 ℃ 20h, to the hydrolysis of red brown.
Neutralization, decolorizing and stirring the hydrolysate to cool, slowly adding 7mol/L NaOH solution, neutralizing to pH3, then adding about 2kg of activated carbon, stirring and keeping the temperature at 70-80 ℃ for 30min to decolorize, the filtrate was filtered to obtain a decolorizing solution. The decolorizing solution was made a light yellow transparent solution.
Detyrosine The decolorizing solution was cooled and stirred, a small amount of tyrosine crystals were added, and allowed to stand for 24h to crystallize tyrosine. The crystals were collected by Suction filtration and washed to obtain crude tyrosine. After refining, the product was obtained and the mother liquor was retained.
Concentration and crystallization the mother liquor was adjusted to pH 2.5 with dilute HCl, and then concentrated under reduced pressure. When a large amount of sodium chloride crystallized out, Suction filtration was performed, and the filtrate was concentrated again until the volume was 10-15L, and suction filtration was performed, the filter cake was combined (mixed crystals of sodium chloride and leucine). The filtrate was adjusted to pH 3.3 with lye, stirred continuously, and added a small amount of glutamic acid as a variety. The glutamic acid was precipitated and crystallized, and the crude glutamic acid was obtained by Suction filtration.
Acid-soluble precipitation the combined filter cake (mixed crystal of sodium chloride and leucine) in the previous step was added with 7.5L of 3mol/L hydrochloric acid solution, heated and stirred, kept at 70-80 ℃ for 0.5h, and filtered with suction to remove sodium chloride crystals, the filtrate is leucine hydrochloride solution, the volume is about 13L, and then according to the volume of 10% to the filtrate is added o-xylene -4-sulfonic acid, so that the complete formation of leucine sulfonate precipitation, filter take filter cake, the filtrate was operated in the same manner, and the filtrate was added with O-xylene -4-sulfonic acid, and then no precipitate was precipitated. The filter cake was combined, stirred with a small amount of distilled water, filtered with suction, and washed twice in this way to obtain leucine sulfonate crystals.
Leucine free leucine sulfonate crystals were added into 7mol/L ammonia water and neutralized to pH6-8, kept at 70-80 ℃ and stirred for 1H, the crystals were collected by Suction filtration and washed twice with a little distilled water to obtain crude leucine.
Recrystallization distilled water was added at a weight ratio of 1/40, and the crude leucine was dissolved by heating, followed by decoloration by adding 1% activated carbon. After the color and clarity of the decolorizing solution were checked to be qualified, it was concentrated under reduced pressure until the volume was 1/4 of the original volume, stirred, cooled, crystallized, and filtered to obtain leucine crystals. The mother liquor was decolorized, concentrated and crystallized again, combined with crystals, and dried to obtain leucine finished product.
raw fish fillets by-product [industrial hydrochloric acid (hydrolysis)]& rarr; Hydrolysate [neutralization and decolorization, 7mol/L NaOH]& rarr;[activated carbon; pH3] transparent liquid [dilute HCl (concentrated crystal)]& rarr;[pH2.5] filter cake [HCl, precipitant (acid-soluble precipitation)]& rarr; precipitate [7mol/L ammonia (ammonolysis)]& rarr;[pH6-8] Crude [distilled water (recrystallization)]& rarr;L-leucine final product.
Take 2kg offal of Hornet fillets by hydrolysis, 5.4L of hydrochloric acid in processing industry, 1.8L of water, the concentration of hydrochloric acid is about 6mol/L, heat preservation 106-110 ℃, hydrolysis 20H to the hydrolysis liquid is red-brown.
Neutralization and decolorization the hydrolysate was stirred and cooled, and neutralized by adding 7mol/L NaOH solution to bring the pH to 3. Then add about 2% of the hydrolysis liquid of activated carbon, heat preservation 70-80 deg C stirring decolorization for half an hour, filter filtrate, yellow transparent liquid.
Concentrate and decolorize the above yellow transparent liquid, adjust the pH to 2.5 with dilute HCl, concentrate under reduced pressure, filter when a large amount of salt crystallizes out, and concentrate the filtrate until the total volume is about 2-3L, filter and combine the filter cake (mixed crystals of NaCl and leucine).
Acid dissolution and precipitation the above combined filter cake was added with 1.5L of 3mol/L HCl solution, heated and stirred, kept at 70-80 ℃ for half an hour, and filtered to discard the NaCl crystals, the filtrate is leucine hydrochloride salt soluble
nutritional supplements; Flavoring and flavoring agents. Preparation of amino acid infusion and comprehensive amino acid preparation, hypoglycemic agent plant growth promoter. According to China's GB 2760-96 can be used as spices. |
amino acid drugs. Used as amino acid infusion and comprehensive amino acid preparation. For the diagnosis and treatment of children with idiopathic hyperglycemia and glucose metabolism disorders, accompanied by decreased bile secretion of liver disease, anemia, poisoning, muscular dystrophy, polio sequelae, neuritis and mental illness. Diabetes, cerebral vascular sclerosis and accompanied by proteinuria and hematuria in patients with kidney disease. Patients with gastric and duodenal ulcer should not be taken. |
is an essential amino acid, which is required for adult men at 2.2g/d. It is necessary for normal growth of infants and maintenance of normal nitrogen balance in adults. The product is used as a nutritional supplement to prepare amino acid infusion and comprehensive amino acid preparation, hypoglycemic agent and plant growth promoter. According to China's GB 2760-86, the product can be used as spices. |
biochemical reagents, belong to the human body essential amino acids, mainly as a nutritional supplement, have hypoglycemic and growth promoting effect. |
nutritional supplements; Flavoring and flavoring agents. Preparation of amino acid infusion and comprehensive amino acid preparation, hypoglycemic agent plant growth promoter. According to China's GB 2760-96 can be used as spices. Used in biochemical research, medicine for the treatment and diagnosis of children with idiopathic hyperglycemia, and for the treatment of anemia, poisoning, muscular atrophy, polio sequelae, neuritis and psychosis. Amino acid drugs. Used as amino acid infusion and comprehensive amino acid preparation. For the diagnosis and treatment of children with idiopathic hyperglycemia and glucose metabolism disorders, accompanied by decreased bile secretion of liver disease, anemia, poisoning, muscular dystrophy, polio sequelae, neuritis and mental illness. Diabetes, cerebral vascular sclerosis and accompanied by proteinuria and hematuria in patients with kidney disease. Patients with gastric and duodenal ulcer should not be taken. Is an essential amino acid, adult men need 2.2g/d, for the normal growth of infants and adults to maintain normal nitrogen balance necessary. The product is used as a nutritional supplement to prepare amino acid infusion and comprehensive amino acid preparation, hypoglycemic agent and plant growth promoter. According to China's GB 2760-86, the product can be used as spices. Used as pharmaceutical raw materials and food additives, biochemical reagents, amino acids are essential to the human body, mainly as a nutritional supplement, have the effect of lowering blood sugar and promoting growth. |
I. Enrichment section
Raw material: steam
The primary mother liquor is passed into the concentration tank, and the steam is introduced, the temperature is 120 degrees, the pressure is -0.09Mpa, the concentration time is 6h, and the crystallization is carried out.
End product: crystallization solution (one neutralization stage)
second, first neutralization
Excipients: sulfuric acid, Pure Water
The crystallization liquid enters the primary neutralization tank, passes into sulfuric acid, pure water, temperature 80, neutralization Time 4H, filters
End product: 1, filtrate (recycling) 2, filter residue (deammonolysis stage)
iii. Aminolysis
Excipients: ammonia water, pure water, steam
The filter residue enters the ammonolysis tank, and ammonia water, pure water, steam, temperature 80, ammonolysis Time 3H, filtration
End product, 1, filtrate (recycling) 2, filter residue (decolorizing section) (cystine)
Four, decolorization section.
Excipients: Steam, pure water, activated carbon
The filter residue enters the decoloring tank and is fed with steam, pure water, activated carbon, temperature 80, decolorization Time 2h, filtration,
End product: 1, filter residue (recycling) 2, filtrate (to secondary neutralization stage)
Five, secondary neutralization segment
Excipients: Ammonia, steam
Filtrate into the secondary neutralization tank, into ammonia, steam, temperature 80, neutralization Time 4H, filtration,
end product, 1, filtrate (recycling) 2, filter residue (I. E., L-leucine crude, derefining section)
Refined segment
Excipients: distilled water, steam (histidine hydrochloride)
Rinse the product of the previous step with distilled water and spin dry it by centrifugation, send it to the dryer, dry it with steam, package it, store it in the warehouse, dry it at a temperature of 100, and dry it for 3H.
End product: L-leucine product
can be used safely in food (FDA,& sect;172.3202000).
Ld505379 mg/kg (rat, subcutaneous).
accounts for 6.4% of the total protein in food (FDA & sect;172.320,2000).
Same as "01115, isoleucine" (FEMA).
l-leucine food flavors the maximum allowable use and the maximum allowable residue in GB 2760 for the preparation of flavor components
FEMA | 3297 | L-LEUCINE |
sublimation point | 145-148°C |
NIST chemical information | information provided by: webbook.nist.gov (external link) |
EPA chemical substance information | information provided by: ofmpeb.epa.gov (external link) |
Introduction | L-leucine (L-leucine), also known as leucine, α-amino-γ-methylpentanoic acid, Α-aminoisohexanoic acid, molecular formula C6H13O2N. Proust was first isolated from cheese in 1819, and later Braconnot crystallized from acid hydrolysate of muscle and wool, and named leucine. |
One of the eight essential amino acids | L-leucine is one of the eight essential amino acids, it belongs to the aliphatic family of amino acids within the twenty protein amino acids, and is called three branched chain amino acids together with L-isoleucine and L-valine. And D-leucine is an enantiomer, white glossy hexahedral crystal or white crystalline powder at room temperature. Odorless and slightly bitter. In the presence of hydrocarbons, the performance is stable in inorganic acid aqueous solution. Each gram is dissolved in 40ml of water and about 100ml of acetic acid. Very slightly soluble in ethanol or ether, soluble in formic acid, dilute hydrochloric acid, Alkaline hydroxide and carbonate solution. L-leucine has the effect of promoting insulin secretion, can lower blood sugar; Promote sleep, reduce sensitivity to pain, relieve migraine, ease anxiety and Nervousness mood , reduce the symptoms of chemical imbalance caused by alcohol in the human body, and help control alcoholism; Have a role in the treatment of dizziness, but also can promote the healing of skin wounds and bone head, so doctors usually recommend leucine supplements for patients after surgery. Often preparation of amino acid infusion and comprehensive amino acid preparation, used in the treatment of or health care; Can also be used as food, cosmetics and feed additives. Plant growth promoters. The best dietary sources of leucine include brown rice, legumes, meat, nuts, soy flour, and whole grains. It should also be noted that excessive intake can also cause side effects , a large number of intake can cause pellagra, vitamin A deficiency, dermatitis, Diarrhea, mental disorders and other problems. Too much leucine in the diet also increases the amount of ammonia in the body and disrupts liver and kidney function. Therefore, patients with impaired liver or kidney function should not be excessively ingested, otherwise it can lead to deterioration of the condition. |
identification test | sublimation at approximately 150 °c. |
content analysis | a sample of about 105 mg, pre-dried at °c for 2H, was accurately weighed and transferred to a ml flask. Add formic acid 3ml, glacial acetic acid 50ml to dissolve. Add 2 drops of crystal violet solution (TS-74) and titrate with 0.1mol/L perchloric acid to a blue-green end point. At the same time, the blank test was carried out and the necessary correction was made. Per Ml of 0.1mol/L perchloric acid corresponds to 13.12mg of L-leucine (C6 H13 NO2). |
toxicity | can be used safely in foods (FDA,§ 172.3202000). Ld505379 mg/kg (rat, subcutaneous). |
usage limit | accounts for 6.4% of the total protein in food (FDA § 172.320,2000). Same as "01115, isoleucine" (FEMA). |
Use | nutritional supplement; Flavoring agent. Preparation of amino acid infusion and comprehensive amino acid preparation, hypoglycemic agent plant growth promoter. According to China's GB 2760-96 can be used as spices. used in biochemical studies, medically in the treatment and diagnosis of idiopathic hyperglycemia in young children, and in the treatment of anemia, poisoning, muscular dystrophy, polio sequelae, neuritis and psychosis. amino acid drugs. Used as amino acid infusion and comprehensive amino acid preparation. For the diagnosis and treatment of children with idiopathic hyperglycemia and glucose metabolism disorders, accompanied by decreased bile secretion of liver disease, anemia, poisoning, muscular dystrophy, polio sequelae, neuritis and mental illness. Diabetes, cerebral vascular sclerosis and accompanied by proteinuria and hematuria in patients with kidney disease. Patients with gastric and duodenal ulcer should not be taken. It is an essential amino acid, and the requirement of adult men is 2.2g/d, which is necessary for normal growth of infants and maintenance of normal nitrogen balance in adults. The product is used as a nutritional supplement to prepare amino acid infusion and comprehensive amino acid preparation, hypoglycemic agent and plant growth promoter. According to China's GB 2760-86, the product can be used as spices. biochemical reagents, which are essential amino acids for human body, are mainly used as nutritional supplements, and have the effects of lowering blood sugar and promoting growth. nutritional supplements; Flavoring and flavoring agents. Preparation of amino acid infusion and comprehensive amino acid preparation, hypoglycemic agent plant growth promoter. According to China's GB 2760-96 can be used as spices. Used in biochemical research, medicine for the treatment and diagnosis of children with idiopathic hyperglycemia, and for the treatment of anemia, poisoning, muscular atrophy, polio sequelae, neuritis and psychosis. Amino acid drugs. Used as amino acid infusion and comprehensive amino acid preparation. For the diagnosis and treatment of children with idiopathic hyperglycemia and glucose metabolism disorders, accompanied by decreased bile secretion of liver disease, anemia, poisoning, muscular dystrophy, polio sequelae, neuritis and mental illness. Diabetes, cerebral vascular sclerosis and accompanied by proteinuria and hematuria in patients with kidney disease. Patients with gastric and duodenal ulcer should not be taken. Is an essential amino acid, adult men need 2.2g/d, for the normal growth of infants and adults to maintain normal nitrogen balance necessary. The product is used as a nutritional supplement to prepare amino acid infusion and comprehensive amino acid preparation, hypoglycemic agent and plant growth promoter. According to China's GB 2760-86, the product can be used as spices. Used as pharmaceutical raw materials and food additives, biochemical reagents, amino acids are essential to the human body, mainly as a nutritional supplement, have the effect of lowering blood sugar and promoting growth. biochemical study. Tissue culture medium was prepared. |
production method | proteins (casein, keratin, etc.) are hydrolyzed with hydrochloric acid or dilute sulfuric acid, the mixture of leucine, L-isoleucine and L-methionine is precipitated from the hydrolysate by alkali neutralization, refined by copper salt method, and L-leucine is precipitated by β-Naphthalene sulfonic acid to obtain a pure product. method 1. Blood Powder [HCl (decomposition)]→[110 ℃, 24h] hydrolysis solution [acid removal] → [vacuum distillation] acid removal solution [activated carbon (adsorption decolorization)]→ effluent [concentration] → [vacuum distillation] concentrate [precipitate] → [O-xylene -4-sulfonic acid] precipitate [ammonia (free)]→ [filtration] crude leucine [activated carbon (decolorization)]→[70 ℃, 1H] filtrate [concentrated crystallization] → [vacuum distillation] L-leucine crude product [water (washing and drying) → L-leucine product hydrolysis, in addition to acid, 500L of 6mol/L HCl solution was added to a 1T hydrolysis tank, and 100kg of animal blood powder was added, heated and incubated at 110-120 ° C. For 24h for reflux hydrolysis, and then concentrated under reduced pressure at 70-80 ° C. To paste. Then, 50L was added and concentrated to a paste form, which was repeated three times, cooled to room temperature, and the filtrate was collected by filtration to obtain a hydrolysate. Adsorption and decolorization the hydrolysate was Diluted 1 times with water and then flowed into the granular activated carbon column (30cm × 180cm) at a flow rate of 0.5L/min until phenylalanine appeared in the effluent, the eluate was washed with deionized water at the same flow rate until the pH of the eluate was 4.0, and the effluent and the Wash were combined to obtain the effluent. Concentration, precipitation and release after concentrating the effluent under reduced pressure to 1/3 of the original volume, 1/10 volume (V/V) of O-xylene-4-sulfonic acid is added under stirring, A precipitate of leucine sulfonate was produced, and the precipitate was taken by filtration, washed twice with 2 volumes of deionized water, and dried by Suction filtration to obtain the leucine sulfonate. Then, the mixture was stirred with 2 volumes of deionized water, and then 6mol/L ammonia water was added to neutralize to pH 6-8, and the mixture was stirred at 70-80 ° C. For 1H to free leucine from its sulfonate. The crystals were cooled, and the crystals were taken by filtration, then washed twice with 2 times the volume of deionized water, and dried by Suction filtration to obtain the crude leucine. After refining, the crude leucine is heated and dissolved in 40 times the volume of deionized water, 0.5% activated carbon (5g/L) is added to keep the temperature at 70 ℃, stirred and decolorized for 1H, and the filtrate is filtered, after concentrating to 1/4 of the original volume, cooling crystallization, The crystals were filtered, washed with a small amount of water, and dried at 70-80 ° C. To obtain a fine L-leucine product. Method 2, using corn gluten as raw material corn gluten [dehydrated and dried] → corn gluten powder [ethanol extraction] → corn gluten [hydrolysis] → hydrolysate [neutralization, decolorization] → decolorization solution [except tyrosine] → filtrate [106-110 ℃, 20h; concentrate] → concentrate [acid-soluble] → precipitate [aminolysis] → Leucine crude [recrystallized] → L-leucine corn gluten powder preparation corn gluten contains a lot of water, solid content is about 20%-30%, the corn gluten powder can only be obtained by dehydration and drying. Corn gluten meal is prepared from corn gluten, extracted with 90%-95% ethanol solution, the extract is evaporated and concentrated to recover ethanol, and then precipitated with water to obtain corn gluten meal. Hydrolysis of corn 10kg, industrial hydrochloric acid 27L, water 9L, into the hydrolysis tank, insulation 106-110 ℃ 20h, to the hydrolysis of red brown. Neutralization, decolorizing and stirring the hydrolysate to cool, slowly adding 7mol/L NaOH solution, neutralizing to pH3, then adding about 2kg of activated carbon, stirring and keeping the temperature at 70-80 ℃ for 30min to decolorize, the filtrate was filtered to obtain a decolorizing solution. The decolorizing solution was made a light yellow transparent solution. Detyrosine The decolorizing solution was cooled and stirred, a small amount of tyrosine crystals were added, and allowed to stand for 24h to crystallize tyrosine. The crystals were collected by Suction filtration and washed to obtain crude tyrosine, The final product is obtained after refining, and the mother liquor is retained. Concentration and crystallization the mother liquor was adjusted to pH 2.5 with dilute HCl, and then concentrated under reduced pressure. When a large amount of sodium chloride crystallized out, Suction filtration was performed, and the filtrate was concentrated again until the volume was 10-15L, and suction filtration was performed, the filter cake was combined (mixed crystals of sodium chloride and leucine). The filtrate was adjusted to pH 3.3 with lye, stirred continuously, and added a small amount of glutamic acid as a variety. The glutamic acid was precipitated and crystallized, and the crude glutamic acid was obtained by Suction filtration. Acid-soluble precipitation the combined filter cake (mixed crystal of sodium chloride and leucine) in the previous step was added with 7.5L of 3mol/L hydrochloric acid solution, heated and stirred, kept at 70-80 ℃ for 0.5h, and filtered with suction to remove sodium chloride crystals, the filtrate is leucine hydrochloride solution, the volume is about 13L, and then according to the volume of 10% to the filtrate is added o-xylene -4-sulfonic acid, so that the complete formation of leucine sulfonate precipitation, filter take filter cake, the filtrate was operated in the same manner, and the filtrate was added with O-xylene -4-sulfonic acid, and then no precipitate was precipitated. Combine the filter cake, stir with a small amount of distilled water, suction filter, This washing was performed twice to obtain the leucine sulfonate crystals. Leucine free leucine sulfonate crystals were added into 7mol/L ammonia water and neutralized to pH6-8, kept at 70-80 ℃ and stirred for 1H, the crystals were collected by Suction filtration and washed twice with a little distilled water to obtain crude leucine. Recrystallization distilled water was added at a weight ratio of 1/40, and the crude leucine was dissolved by heating, followed by decoloration by adding 1% activated carbon. After the color and clarity of the decolorizing solution were checked to be qualified, it was concentrated under reduced pressure until the volume was 1/4 of the original volume, stirred, cooled, crystallized, and filtered to obtain leucine crystals. The mother liquor was decolorized, concentrated and crystallized again, combined with crystals, and dried to obtain leucine finished product. Method 3. Using the raw material of the raw material of the fish fillets [industrial hydrochloric acid (hydrolysis)]→ hydrolysate [neutralization and decolorization, 7mol/L NaOH]→ [activated carbon; pH3] transparent liquid [dilute HCl (concentrated crystal)]→[pH2.5] filter cake [HCl, precipitant (acid-soluble precipitation)]→ precipitate [7mol/L ammonia (ammonolysis)]→[pH6-8] Crude [distilled water (recrystallized)]→ L-leucine finished product. Take 2kg offal of Hornet fillets by hydrolysis, 5.4L of hydrochloric acid in processing industry, 1.8L of water, the concentration of hydrochloric acid is about 6mol/L, heat preservation 106-110 ℃, hydrolysis 20H to the hydrolysis liquid is red-brown. Neutralization and decolorization the hydrolysate was stirred and cooled, and neutralized by adding 7mol/L NaOH solution to bring the pH to 3. Then add about 2% of the hydrolysis solution of activated carbon, heat preservation 70-80 ℃, stirring and decoloring for half an hour, filter to take the filtrate, Yellow transparent liquid was obtained. Concentrate and decolorize the above yellow transparent liquid, adjust the pH to 2.5 with dilute HCl, concentrate under reduced pressure, filter when a large amount of salt crystallizes out, and concentrate the filtrate until the total volume is about 2-3L, filter and combine the filter cake (mixed crystals of NaCl and leucine). Acid dissolution and precipitation the above combined filter cake was added with 1.5L of 3mol/L HCl solution, heated and stirred, kept at 70-80 ℃ for half an hour, and filtered to discard the NaCl crystals, the filtrate is leucine hydrochloride salt soluble with dry hemoglobin as raw material in sulfuric acid reflux for several hours, alkali neutralization precipitation, filtration, crystallization, the product was treated with concentrated hydrochloric acid and sodium 2-bromotoluene-5-sulfonate, washed with ether after hydrolysis and crystallized. The hydrochloric acid or dilute sulfuric acid hydrolysis solution of the protein (casein, keratin, etc.) is neutralized with an alkali to precipitate leucine. This precipitate was mixed with L-isoleucine and L-methionine, purified by a copper salt method, and precipitated with β-Naphthalene sulfonic acid to obtain pure crystals of L-leucine. |
toxic substance data | information provided by: pubchem.ncbi.nlm.nih.gov (external link) |