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GB 1886.324-2021: National food safety standard - Food additives - Metatartaric acid
GB 1886.324-2021
National food safety standard-Food additives-Metatartaric acid
National Standards of People's Republic of China
National Food Safety Standard
Food additive metatartaric acid
Released on 2021-02-22
2021-08-22 implementation
National Health Commission of the People's Republic of China
Issued by the State Administration for Market Regulation
National Food Safety Standard
Food additive metatartaric acid
1 Scope
This standard applies to tartaric acid as raw material, baking at 168℃~172℃ for 3.5h, or heating to 180℃~190℃, and then natural
The food additive metatartaric acid prepared by cooling.
2 Chemical name, molecular formula, structural formula and relative molecular mass
2.1 Chemical name
Metatartaric acid
2.2 Molecular formula
C8H8O10
2.3 Structural formula
2.4 Relative molecular mass
264.142 (according to.2018 international relative atomic mass)
3 Technical requirements
3.1 Sensory requirements
Sensory requirements should meet the requirements of Table 1.
Appendix A
Testing method
Warning. Some test procedures specified by the test method may lead to dangerous situations. The operator should take appropriate safety and protective measures.
A.1 General provisions
Unless otherwise specified, only use reagents confirmed to be analytically pure and the tertiary water specified in GB/T 6682 in the analysis. Test method
The solutions, preparations and products used are prepared in accordance with GB/T 601, GB/T 602 and GB/T 603 unless other requirements are specified.
A.2 Identification test
A.2.1 Reagents and materials
A.2.1.1 Sulfuric acid solution. c(H2SO4)=0.0025mol/L.
A.2.1.2 Microporous membrane. 0.22μm.
A.2.2 Instruments and equipment
A.2.2.1 High performance liquid chromatograph, diode array detector.
A.2.2.2 Analytical balance. Sensitivity 0.0001g.
A.2.2.3 Micro-injector. 10μL.
A.2.3 Reference chromatographic conditions
A.2.3.1 Chromatographic column. RezexROA-OrganicAcid, 300mm×7.8mm, 8μm, or other chromatographic columns that meet the conditions.
A.2.3.2 Column temperature. 40℃.
A.2.3.3 Mobile phase. 0.0025mol/L sulfuric acid solution.
A.2.3.4 Flow rate. 0.4mL/min.
A.2.3.5 Injection volume. 10μL.
A.2.3.6 Detection wavelength. 210nm.
A.2.4 Analysis steps
A.2.4.1 Preparation of 0.0025mol/L sulfuric acid solution
Add 800mL ultrapure water to a 1000mL beaker, slowly add 136μL 98% concentrated sulfuric acid, stir slowly with a glass rod, and wait.
After the solution is cooled to room temperature, transfer the prepared solution into a 1000mL volumetric flask and dilute the volume to 1000mL.
A.2.4.2 Solution preparation
Weigh 0.010g of the sample to be tested, put it into a 50mL beaker, add 30mL of 0.0025mol/L sulfuric acid solution, and stir to
After the sample is completely dissolved, transfer it to a 100mL volumetric flask, and dilute to 100mL with 0.0025mol/L sulfuric acid solution.
A.2.4.3 Determination
After taking 10mL of the prepared sample solution through a 0.22μm filter membrane, take 10μL of the processed sample solution and inject it into the liquid chromatograph.
Perform high performance liquid chromatography analysis, record the retention time of the chromatographic peak, and judge whether it is metatartaric acid according to the retention time. Metatartaric acid in a given
Under chromatographic conditions and reagent conditions, the retention time is 10.0min. See Figure A.1.
Figure A.1 Liquid chromatogram of metatartaric acid
A.3 Determination of total acid content (calculated on a dry basis) and degree of decarboxylation
A.3.1 Reagents and materials
A.3.1.1 Bromothymol blue solution. 4.0g/L.
A.3.1.2 Sodium hydroxide standard titration solution. c(NaOH)=1.0mol/L.
A.3.1.3 Sulfuric acid solution. c(H2SO4)=0.5mol/L.
A.3.2 Analysis steps
Weigh 2.000g sample, add 100mL deionized water and heat to dissolve it for later use. Take 50mL of the newly prepared metatartaric acid solution and put it in
In a 250mL Erlenmeyer flask, add 3 drops of bromothymol blue indicator, and titrate with 1.0mol/L sodium hydroxide solution until the solution is blue-green and stable.
The color does not change for 30s, and the consumption volume V1 of sodium hydroxide is recorded. Continue to add 20.0mL 1.0mol/L sodium hydroxide solution and cap the bottle
Stopper, let stand for 2h at room temperature, then titrate the excess sodium hydroxide with 0.5mol/L sulfuric acid until the solution is blue-green, and record the consumption of sulfuric acid
量V2.
Before the measurement, the test sample needs to be dried in an oven at 120°C to a constant weight before weighing.
A.3.3 Result calculation
Each consumption of 1.0mL1.0mol/L sodium hydroxide solution is equivalent to 0.075g tartaric acid in the solution.
The total acid content (including free and decarboxylated acid) w in the sample to be tested is calculated according to formula (A.1).
w=[0.075×(V1 20.0-V2)]/m×100% (A.1)
Where.
w ---Total acid content,% (retain three significant figures);
0.075 --- conversion factor;
V1 --- The volume of sodium hydroxide used in the first titration, in milliliters (mL) (the reading is accurate to 0.1mL);
20.0 --- The amount of sodium hydroxide solution added after the first titration, in milliliters (mL) (the reading is accurate to 0.1mL);
V2 --- The volume of sulfuric acid used in the second titration, in milliliters (mL) (the reading is accurate to 0.1mL);
m ---The mass of the sample weighed, in grams (g).
The degree of decarboxylation T of the sample to be tested is calculated according to formula (A.2).
T=(20.0-V2)/(V1 20.0-V2)×100% (A.2)
Where.
T ---Decarboxylation degree,% (retain three significant digits);
20.0 --- The amount of sodium hydroxide solution added after the first titration, in milliliters (mL) (the reading is accurate to 0.1mL);
V2 --- The volume of sulfuric acid used in the second titration, in milliliters (mL) (the reading is accurate to 0.1mL);
V1 --- The volume of sodium hydroxide used in the first titration, in milliliters (mL) (the reading is accurate to 0.1 mL).
For the above determinations, the arithmetic average of the results of two parallel determinations is taken as the report result. The absolute difference between the two parallel determination results is not greater than
0.2%.
A.4 Oxalate test
A.4.1 Reagents and materials
A.4.1.1 Ammonia solution. 10%.
A.4.1.2 Calcium sulfate saturated solution.
A.4.2 Analysis steps
Weigh 1.00g sample, dissolve it in 10mL water, neutralize it with ammonia solution to neutrality, add 10mL calcium sulfate saturated solution, shake well
Observe, there must be no turbidity.
A.5 Sulfate test
A.5.1 Reagents and materials
A.5.1.1 Hydrochloric acid solution. 14.
A.5.1.2 Barium chloride solution. Weigh 12.0g BaCl2·2H2O and dissolve it in 100mL water.
A.5.2 Analysis steps
Weigh 1.00g sample, dissolve it in 100mL water, and heat to dissolve. Take 10mL of this solution and place it in a test tube, add 3 drops of hydrochloric acid solution
And 1mL barium chloride solution, shake well and observe, there should be no turbidity.