Chapter 1: Overview of Monodiseryl Tartrates
Aliases and encodings
Aliases: mono and diglycerides diacetyl tartaric acid, DATAM. Encoding: CNS 10.010; INS 472e.
chemical structure
R1: Fatty acid group
R2, R3: can be a fatty acid group or a fatty acid group and a hydrogen.
Physical properties
Depending on the iodine value of the oil used in the preparation, it can be a viscous liquid fat sample or a waxy solid, and a 10% anti-caking agent can be made into a white powder with a slightly sour odor. Soluble in any proportion in most grease solvents, soluble in methanol, propanol, ethyl acetate, but not soluble in other alcohols, acetic acid and water, dispersed in water, and resistant to hydrolysis for an appropriate long time. The pH of the 3% aqueous dispersion solution of this product is 2~3.
Functional role
Emulsifiers, thickeners.
Quality standards
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project
index
GB25539-2010
JECFA(2009)
FCC(7)
Tartaric acid (after saponification)/%
Acetic acid (after saponification)/%
Acid number/(mgKOH/g)
Free fatty acids/%
Total fatty acids/% ≥
Glycerol (after saponification)/% ≥
Free glycerol/% ≤
铅/（mg/kg） ≤
Burn residue/% ≤
Saponification value /(mgKOH/g)
Sulfate ash/% ≤
10-40
8-32
In line with the claim
-
11-28
2.0
0.5
40-130
17.0-20.0
14.0-17.0
62-76
56.0
12
380-425
Toxicological basis
LD50 rats are taken orally greater than 10 g/kg (bw).
GRAS FAD-21CFR 184.1101。
ADI 0~50mg/kg(bw)(JECFA,1994)。
use
(1) GB 2760-2011 "National Standard for Food Safety" The scope of use and dosage of food additives are described in page 782.
(2) Actual use reference:
(1) Used in bread, the quality of bread can be improved, especially when combined with single glycerides. Mono-diglycerides of diacetyl tartaric acid can make the bread produced beautiful in appearance, the internal tissue structure is fine, and the preservation period is long.
(2) As one of the active ingredients of the blowing agent used in cake making, it can improve the traditional mixing and beating of eggs, sugar and flour together, simplifying the operation and shortening the stirring time, which only takes 5-7 minutes.
(3) For margarine, cold drinks, cream, can make the cream soft and delicate, the amount of use is about 10g/kg.
Chapter 2 National Standards and Regulations on Food Safety
2.1 Scope
This standard applies to the food additive mono and diglycerides of biacetylate tartaric acid prepared by the reaction of biacetyl tartaric anhydride with mono and bi fatty acid glycerides.
2.2 Normative reference documents
The documents referenced in this standard are essential for the application of this standard. For references to dates, only the version of the date indicated applies to this Standard. For undated references, the latest version (including all amendments) shall apply to this Standard.
2.3 Technical Requirements
2.3.1 Sensory requirements: should comply with the provisions of Table 2-1.
Table 2-1 Sensory requirements
request
Inspection methods
Color
Light yellow or milky white
Take an appropriate amount of sample in a clean, dry white porcelain bottle or beaker, in natural light, observe its color and tissue state, and smell it.
smell
It has a sour taste
Organization status
At room temperature, liquid, paste or waxy solids
2.3.2 Physical and chemical indicators: should comply with the provisions of Table 2-2.
Table 2-2 Physicochemical indicators
Total tartaric acid, w%
4.2
Total glycerol, w%
4.3
Total acetic acid, w%
4.4
Free glycerin, w% ≤
4.5
Burn residue, w% ≤
GB/T 9741
铅（pb）/(mg/g)≤
GB 5009.12
Acid number/(mg/g)
4.6
Saponification value/(mg/g)
4.7
Sample weighing volume is about 5g.
Chapter 3 Preparation Methods
3.1 Method 1
1kg L-tartaric acid and 2.2kg acetic anhydride were pumped into the reactor, 5g of acetic acid and 10g of benzalkonium bromide were added, stirred evenly, and reacted for 2 hours under the condition of 75 degrees Celsius to give an intermediate product containing biacetyl tartaric anhydride; The reaction under the condition of vacuum degree of 0.08MPa is 3 hours, cooling after the end of the reaction, distillation, 4.62kg final product is obtained, the content of mono and diglycerides of biacetylate tartaric acid is 84.3%, the acid value is 67, and the saponification value is 402.The physical and chemical indicators of mono and diglycerides of biacetyl tartaric acid are in line with the relevant requirements of GB 25539-2010 "Food Additives Mono and Diglycerides of Diacetylate Bitartrate".
3.2 Method 2
1kg L-tartaric acid and 2.5kg acetic anhydride were pumped into the reactor, 10g of acetic acid and 15g of benzalkonium bromide were added, stirred evenly, reacted for 2 hours under the condition of 70 degrees Celsius, and the intermediate product containing diacetyl tartaric anhydride was obtained; Under the condition of vacuum degree of 0.07MPa, the reaction is 3 hours, the temperature is cooled after the reaction is completed, refined, and the final product of 4.41kg is obtained, and the physical and chemical indicators of mono and diglycerides of biacetylate tartaric acid are in line with the relevant requirements of GB 25539-2010 "Food Additives Mono and Diglycerides of Diacetylate Bitartrate", which are dried by spray to obtain a white powder.
3.3 Method Three
1kg L-tartaric acid and 2kg of acetic anhydride were pumped into the reactor, 10g of acetic acid and 15g of benzalkonium bromide were added, stirred evenly, reacted for 1 hour under the condition of 80 degrees Celsius, and the intermediate product containing diacetyl tartaric anhydride was obtained; 2.2kg of monostearate glyceride was added to the intermediate product, stirred well, at 120 degrees Celsius, The reaction was 1.5 hours under the condition of vacuum 0.09MPa, cooled down after the end of the reaction, distilled, and 4.49kg of final product was obtained, the content of mono and diglycerides of biacetylate tartaric acid was 84.8%, the acid value was 66, and the saponification value was 396. The physical and chemical indicators of mono and diglycerides of biacetylate tartaric acid are in line with the relevant requirements of GB 25539-2010 "Food Additives Diacetyl Tartaric Acid Mono and Diglycerides", which are spray dried to obtain a white powder.
Comparison method 1: 1kg L-tartaric acid and 2kg acetic anhydride were pumped into the reactor, 10g of acetic acid was added, stirred evenly, and the reaction was carried out for 2 hours under the condition of 100 degrees Celsius to obtain an intermediate product containing biacetyl tartaric anhydride; 2.2kg of monostearate glyceride and 15g of benzalkonium bromide were added to the intermediate product, and stirred evenly, at 115 degrees Celsius, vacuum 0. The reaction was carried out for 2 hours under the condition of 09MPa, cooled down after the end of the reaction, distilled, and 4.27kg of final product was obtained, and the content of mono and diglycerides of biacetylate bitartrate was 72.5, the acid number was 75, and the saponification value was 404.
Comparison method two: 1kg L-tartaric acid and 2.2kg acetic anhydride pumped into the reactor, add 5g of acetic acid and 10g of polyethylene glycol ether, stir well, 75 degrees Celsius under the condition of reaction for 2 hours to obtain an intermediate product containing biacetyl tartaric anhydride; add 2.5kg of monostearate glyceride to the intermediate product, stir well, at 110 degrees Celsius, The reaction was carried out for 3 hours under the condition of vacuum 0.08MPa, cooled down after the end of the reaction, distilled, and the final product of 4.09kg was obtained, and the content of mono and diglycerides of biacetylate bitartrate was 70.3, the acid value was 77, and the saponification value was 412.
Chapter 4: Measurement Methods
4.1 Identification experiments
4.1.1 Reagents and Materials
(a) Ethanol
(b) Ethanol lead test solution: weigh 9.5g of lead acetate crystals [Pb(C2H2O2)2•••••3H2O], dissolve in freshly boiled and cooled water, and set the volume to 100ml.
4.1.2 Determination
Weigh 0.5g of the sample, dissolve in 10 ml of ethanol, add lead acetate test solution dropwise, should generate a white flocculent almost insoluble precipitate of water.
4.2 Determination of total tartaric acid
4.2.1 Reagents and Materials
(a) Trichloromethane (chloroform).
(b) Tartaric acid
(c) Acetic acid
(d) Sodium metavanadate solution: 50g/L
(e) Potassium hydroxide solution: 0.5mol/L
(f) Phosphoric acid solution: 1 + 4.
(g) Phthalate indicator solution: 10g/L.
4.2.2 Instruments and Equipment
(a) Spectrophotometer or photochromimeter equipped with a 520 nm filter.
(b) Air condenser with a length of 65 cm or more.
4.2.3 Analysis Steps
4.2.3.1 Drawing of standard curves
Weigh about 0.1 g of tartaric acid (accurate to 0.001 g), dissolve with water and set the volume to 100 mL, mix well. Accurately aspirate 0mL, 3.0mL, 4.0mL, 5.0mL, 6.0mL of the solution, placed in a 25mL colorimetric tube, and then add water to fix the volume to 10mL. Add 4.0 mL of freshly prepared sodium metavanadate solution and 1.0 mL of acetic acid to each cuvette. Set the absorbance of the blank sample to zero and determine the absorbance of the above tartaric acid solution at a wavelength of 520 nm (Note: These solutions are determined within 10 min after color development).
The obtained data, with absorbance as the ordinate coordinate and the mass of the corresponding tartaric acid (in mg) as the abscissa, draw the standard curve.
4.2.3.2 Preparation of sample solutions
Weigh about 4 g of the specimen (accurate to 0.001 g), transfer to a 250 mL Erlenmeyer flask, and add 80 mL of potassium hydroxide solution at a concentration of 0.5 mol/L and 0.5 mL of phenolphthalein indicator solution. Attach an air condenser with a length of more than 65 cm to the Erlenmeyer flask and heat the mixture on a heating rod for about 2. 5 hours. Add the phosphoric acid solution while hot until the Congo red test strip is significantly acidic. Reconnect the air condenser and heat until the fatty acids are liquefied and become clear. After the mixture has cooled, a small amount of water and chloroform are added, the mixture is transferred to a 250mL dispensing funnel 1, free fatty acids are extracted with chloroform, each time with 25mL, 3 times in a row, the extract is concentrated in another dispensing funnel 2, wash the extract in the dispensing funnel 2 with water, each time with 25mL, 3 times continuously, the lotion is incorporated into the dispensing funnel 1 containing the aqueous phase layer. Transfer all the aqueous phase layers in the dispensing funnel 1 into a 250 mL beaker, heat it on a steam bath to remove trace amounts of chloroform, and then filter it into a 500 mL volume flask by an pickled precision filter paper, dilute with water and set the volume to the scale. Keep the remaining solution1 for determination of total glycerol content.
4.2.3.3 Determination
Accurately aspirate solution 2 prepared in the 10 mL analysis step, place it in a 25 mL cuvette, and then start the operation according to the analysis step of "Drawing of Standard Curves" to obtain the absorbance of the sample solution. The mass of tartaric acid in solution 2 is obtained according to the standard curve.
4.2.4 Calculation of results
The total tartaric acid content X1 is calculated according to equation 1:
…………………………………… （1）
where:
X1- Total tartaric acid content, %;
m- According to the absorbance and standard curve of the sample solution, the mass of tartaric acid in solution 2 obtained is mg;
20-dilution multiple;
Mass of M1-specimen in mg;
The experimental results are based on the arithmetic average of the parallel determination results. The difference between the results of the two independent assays obtained under reproducible conditions is not more than 1%.
4.3 Determination of total glycerol
4.3.1 Reagents and Materials
(a) Glacial acetic acid
(b) periodic acid solution; 2.7g of periodic acid is dissolved in 50ml of water, 950ml of glacial acetic acid is added, and mixed thoroughly, this solution needs to be stored away from light.
(c) Potassium iodide solution;
(d) Standard titration solution of sodium thiosulfate;
(e) Starch indicator solution; 10 g/L.
4.3.2 Analysis Steps
Accurately aspirate 5 ml of total tartaric acid content of solution 1, this 5 ml solution 1 is the sample solution, pipette the sample solution into a 250 ml glass stopper Erlenmeyer flask or iodine bottle. Add 15 ml of glacial acetic acid and 25 ml of periodic acid solution to the bottle, shake the mixture for 1-2 minutes, let stand for 15 minutes, then add 15 ml of potassium iodide solution and 15 ml of water, shake well and let stand for 1 minute, titrate free iodine with sodium thiosulfate standard titration solution, with starch indicator solution as an indicator. Blank sample titration with water instead of sample solution. The blank-corrected volume is the sodium thiosulfate consumed to titrate the glycerol and tartaric acid contained in the sample in 5 ml solution 1.
4.4 Determination of total acetic acid
4.4.1 Reagents and Materials
(a) Perchloric acid solution, about 4mol / L.
(b) Phenolphthalein indicator, 10 g/L.
(c) Sodium hydroxide standard solution, 0.5 mol/L.
4.4.2 Instruments and Equipment
(a) Hortvet-Sellier distillation instrument
(b) Sellier inner tubes and large distillation traps
4.4.3 Analysis Steps
Weigh about 4 g of the specimen (accurate to 0.001 g), transfer to the inner tube of the distillation instrument, and insert the inner tube into an outer bottle, about 300 mL of hot water that has just been heated to boiling hot water, and add 10 mL of perchloric acid solution with a concentration of about 4 moL/L to the sample. Connect the inner tube to a water-cooled condenser by distillation well, distill by heating the outer bottle, collect 100 mL of distillate in 20-25 minutes, collect several 100 mL of distillate, add a phenolphthalein indicator to each sample solution, titrate with sodium hydroxide standard solution, continue distillation until the collected 100 mL distillate requires less than 0.5 mL of sodium hydroxide standard solution to neutralize.
4.4.4 Calculation of results
The content of total acetic acid X3 is calculated according to equation 2:
…………………………………… （2）
X3- Total acetic acid content, %;
V3- Continuous titration consumes the total volume of sodium hydroxide standard solution in milliliters (mL);
Actual concentration of C3-sodium hydroxide standard solution in moles per liter (mol/L)
60.06- Consume 1 ml of 1.0mol/L sodium hydroxide standard solution equivalent to 60.06 mg of acetic acid;
Mass of m3-specimens in milligrams (mg).
The experimental results are based on the arithmetic average of the parallel determination results. The difference between the results of the two independent assays obtained under repetitive conditions is not more than 2%.
Chapter 5: Effects on Frozen Dough
5.1 Effect on the tensile properties of frozen dough
Frozen dough is the use of the principle of freezing, the semi-finished products, that is, bread dough below -18 degrees Celsius frozen and refrigerated. In addition to producing bread, frozen dough can also be processed into traditional foods in China, such as steamed buns, spring rolls, buns, dumplings, etc. The quality of frozen dough is closely related to the protein content and quality of flour, the formulation of the dough and the gluten hydration ability of the dough during the freezing process, enzyme activity, the degree of protein denaturation, the frost resistance of yeast cells and the quality of flour.
5.1.1 Determination of tensile properties of frozen dough
By changing the amount of various additives added to the frozen dough, using the texture analyzer to test the tensile resistance of the frozen dough, the tensile force (g) - tensile distance (mm) curve is obtained, and the qualitative and quantitative analysis of the curve obtains the optimal ratio of each component.
5.1.1.1 Test steps
(1) And noodles: mix the ingredients with good ratios evenly, put them into the noodle machine, and the noodles for 15 minutes, and the final temperature is controlled at about 20 degrees Celsius. (2) Wake up: Put the reconciled dough into the plastic bag immediately and let it rise for 15 minutes. (3) Freezing: Put the waking dough in a -22 degree Celsius refrigerator and freeze for 24 hours. (4) Thawing: Thaw at 33 degrees Celsius for 1 hour.
5.1.1.2 Test conditions
探头：Spaghetti/Noodle Tensile Rig Code A/SPR
Mould: Tensile
Pre-test speed 1mm/s
Test speed 1mm/s
Post-test speed 10mm/s
Trigger distance 50mm
Data processing: Response surface analysis with Design expert software.
5.1.2 Results and discussion of the tensile properties of frozen dough
5.1.2.1 Effect of additive dosage on stretch area of frozen dough
The tensile resistance of the frozen dough can reflect the stability of the internal structure. Use the stretch area as an indicator to reflect the tensile resistance of the dough, the larger the stretch area, the better the tensile resistance of the dough, and the better its stability. The trend of additive addition to frozen dough tensileity is shown in Figure 1.
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