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National Food Safety Standard -- Food Nutrition Enhancer -- Calcium Citrate-malate
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GB 1903.18-2016
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Basic data | Standard ID | GB 1903.18-2016 (GB1903.18-2016) | | Description (Translated English) | National Food Safety Standard -- Food Nutrition Enhancer -- Calcium Citrate-malate | | Sector / Industry | National Standard | | Classification of Chinese Standard | X09 | | Classification of International Standard | 67.040 | | Word Count Estimation | 8,891 | | Date of Issue | 2016-12-23 | | Date of Implementation | 2017-06-23 | | Regulation (derived from) | National Health and Family Planning Commission Notice No.17 of 2016 | | Issuing agency(ies) | National Health and Family Planning Commission of the People's Republic of China, State Food and Drug Administration | | Summary | This standard applies to calcium carbonate and other calcium sources, citric acid, malic acid as raw materials, according to a certain percentage of mixed reaction after the neutralization, precipitation, separation, filtration and drying process and the preparation of food nutrition enhancers citric acid malic acid calcium. |
GB 1903.18-2016: National Food Safety Standard -- Food Nutrition Enhancer -- Calcium Citrate-malate ---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
(Food safety national standard food nutrition enhancer citric acid malate calcium)
National Standards of People's Republic of China
National standards for food safety
Food Nutrition Enhancers Calcium Citrate Calcium Malate
2016-12-23 released
2017-06-23 Implementation
National Health and Family Planning Commission of the People's Republic of China
State Food and Drug Administration issued
National standards for food safety
Food Nutrition Enhancers Calcium Citrate Calcium Malate
1 Scope
This standard applies to calcium carbonate and other calcium sources, citric acid, malic acid as raw materials, according to a certain proportion of mixed reaction after the neutralization, precipitation, separation,
Filtration and drying process and the production of food nutrition enhancer citric acid malate calcium.
2 chemical name, molecular formula, structural formula
2.1 Chemical name
Calcium citrate Calcium citrate
2.2 Molecular formula
Cax (C6H5O7) y (C4H4O5) z · nH2O
2.3 Structural formula
Taking Ca6 (C6H5O7) 2 (C4H4O5) 3 · 5H2O as an example, the structure is as follows.
Ca6 (C6H5O7) 2 (C4H4O5) 3 · 5H2O
3 technical requirements
3.1 sensory requirements
Sensory requirements shall comply with the requirements of Table 1.
Table 1 sensory requirements
The project requires a test method
Color white
State powder crystals
Take the appropriate amount of sample in a clean, dry white porcelain dish
Under the light, observe the color and state
3.2 Physical and chemical indicators
Physical and chemical indicators should be consistent with the provisions of Table 2.
Table 2 Physical and chemical indicators
Item Index Test Method
Citrate calcium malate content (Ca, dry basis), w /% 20 ~ 26 Appendix A A.4
pH (100g/L) 5 ~ 8 Appendix A A.5
Loss on drying, w /% ≤ 10 Appendix A A.6
Hydrochloric acid insoluble matter, w /% ≤ 0.2 Appendix A A.7
Solubility, w /% ≥ 80 Appendix A, A.8
Fluoride (in terms of F)/(mg/kg) ≤ 50 GB/T 5009.18
Heavy metals (Pb)/(mg/kg) ≤ 10 GB 5009.74
Lead (Pb)/(mg/kg) ≤ 2.0 GB 5009.12
Total arsenic (in As)/(mg/kg) ≤ 2.0 GB 5009.11
Appendix A
Testing method
A.1 Warning
Some of the reagents used in this standard test procedure are corrosive and require careful operation such as splashing into the skin.
Rinse, severe treatment immediately. The use of drugs, should be strictly in accordance with the relevant provisions of management; use should avoid inhalation or contact with the skin, must
Should be carried out in a fume hood. Exposed parts of the wound can not touch.
A.2 General provisions
The reagents and water used in this standard test method, when not specified in other requirements, refer to the analytical reagent and the third grade specified in GB/T 6682
water. Standard solution used in the test, the standard solution of impurities, preparations and products, in the absence of other requirements, according to GB/T 601,
GB/T 602, GB/T 603. The solution used in the test refers to the aqueous solution when it is not specified in the formulation of the solvent.
A.3 Identification test
A.3.1 Reagents and materials
A.3.1.1 Ammonia solution. (2 3, volume ratio).
A.3.1.2 p-Aminobenzenesulfonic acid. 10 g/L.
A.3.1.3 Sodium hydroxide solution. 40 g/L.
A.3.1.4 sodium nitrite solution..200 g/L.
A.3.2 Malate Root Identification
Weigh the sample 0.5g, accurate to 0.01g. Placed in 50mL test tube, add water 10mL dissolved. Neutralized with ammonia solution to neutral, plus
1 mL of p-aminobenzenesulfonic acid solution and heated in a boiling water bath for 5 min. Add sodium nitrite solution 5mL, and then placed in a water bath for 3min
After adding sodium hydroxide solution 5mL, the test solution should be immediately color.
A.3.3 Qualitative identification of infrared spectroscopy
Potassium bromide compression method, in accordance with the provisions of GB/T 6040 test, the infrared spectrum of the sample should be consistent with the control spectrum. Correct
The spectrum is shown in Appendix B.
A.4 Determination of calcium citrate content (Ca, dry basis)
A.4.1 Methodological Summary
In the test solution, a small amount of magnesium ions as the auxiliary indicator, that is, magnesium ions and chromium black T generated a stable complex indicates the color change,
Titration with ethylenediamine tetraacetic acid disodium (EDTA) standard titration solution, according to ethylenediamine tetraacetic acid disodium (EDTA) standard titration solution consumption
Calculate the calcium content.
A.4.2 Reagents and materials
A.4.2.1 hydrochloric acid solution (14, volume ratio).
A.4.2.2 Ammonia-ammonium chloride buffer solution (pH ≈ 10).
A.4.2.3 zinc oxide reference reagent (purity not less than 99.9%).
A.4.2.4 Magnesium Sulfate Solution (120 g/L).
A.4.2.5 Chromium Black T (5 g/L).
A.4.2.6 Disodium ethylenediamine tetraacetate (EDTA) standard titration solution. c (EDTA) ≈0.05mol/L.
Ethylenediamine tetraacetic acid disodium standard titration solution preparation. Weigh 20gEDTA, dissolved in water, diluted with water to 1000mL, shake.
Calibration. accurately weighed 0.15g by 800 ℃ ± 50 ℃ in the high temperature furnace to the constant weight of the zinc oxide reference reagent (A.4.2.3), with less
The amount of water wetting, add 2mL hydrochloric acid solution (20%) dissolved, add 100mL water, with ammonia solution (10%) to adjust the solution pH to 7 ~ 8, plus
10 mL ammonia-ammonium chloride buffer solution (pH ≈ 10) and 5 drops of chromium black T solution, titrated with a solution of EDTA solution to the solution by purple
For pure blue. At the same time as a blank test.
EDTA standard titration solution concentration, the unit is mol per liter (mol/L), according to formula (A.1) calculation.
c (EDTA) =
m × 1000
(V1-V) x M
(A.1)
Where.
m - the mass of the zinc oxide reference reagent in grams (g);
V1 - consumption of EDTA standard solution in milliliters (mL);
V - blank consumption of EDTA standard solution in milliliters (mL);
M - the molar mass of zinc oxide in grams per mole (g/mol) [M (ZnO) = 81.39 g/mol];
1000 --- conversion factor.
A.4.2.7 Ammonia solution (10%).
A.4.3 Analysis steps
2 drops of magnesium sulfate solution, add ammonia - ammonium chloride buffer 15mL, plus chromium black T indicator solution 2 drops, with EDTA standard solution titration to
Pure blue; another dry sample after about 0.35g, accurate to 0.0001g, add water 30mL to dissolve, add triethanolamine 5 drops, and
With the above titration of magnesium sulfate solution, and then EDTA standard solution titration, to the color from purple to pure blue is the end point. with
Do blank test.
A.4.4 Calculation of results
Calcium citrate content (Ca, dry basis) of the mass fraction w1, calculated according to formula (A.2).
w1 =
(V-V0) × c × M
1000 × m ×
100% (A.2)
Where.
V --- sample consumption EDTA standard solution titration volume, in milliliters (mL);
V0 --- blank test consumption EDTA standard solution titration volume, in milliliters (mL);
c - the concentration of EDTA standard solution in moles per liter (mol/L);
M - the molar mass of calcium in grams per mole (g/mol) [M (Ca) = 40.1 g/mol];
m --- sample quality, in grams (g);
1000 --- conversion factor.
The results of the test are based on the arithmetic mean of the parallel measurement results (1 decimal place is reserved). Two independent tests obtained under repetitive conditions
The absolute difference of the result is not more than 5% of the arithmetic mean.
A.5 Determination of pH
Take 10.0g sample, add water 100mL stirring dissolved, to be clarified, and then according to the provisions of GB/T 9724 measured sample solution pH.
A.6 Determination of dry weight loss
A.6.1 Reagents and materials
A.6.1.1 weighing bottle. diameter 40mm × 25mm.
A.6.1.2 Analyze the balance.
A.6.1.3 Dryers.
A.6.1.4 Oven.
A.6.2 Analysis steps
Weigh the sample 1g ~ 2g, accurate to 0.0001g, placed in the 150 ℃ ± 5 ℃ drying oven to the already constant weight of the weighing bottle
in. Such as the sample for the larger crystal or block, should be quickly crushed to the diameter of 2mm below the powder, the sample in the weighing bottle in the thickness of a layer
Not more than 5mm. The flask was placed in a drying oven at 150 ° C ± 5 ° C for 4 hours, placed in a desiccator and cooled to room temperature.
Weighing many times until constant weight (before and after the two weighing results difference is not greater than 2mg).
A.6.3 Calculation of results
The mass fraction w2 of dry weight loss is calculated according to formula (A.3)
w2 =
m1-m2
m1-m x
100% (A.3)
Where.
m --- weighing the quality of the bottle, in grams (g);
m1 --- weighing bottle with the quality of the sample, in grams (g);
m2 --- the quality of the bottle and the sample after drying, in grams (g).
The arithmetic mean of the parallel measurement results is the result of the measurement, and the difference between the two parallel measurements does not exceed 5% of the arithmetic mean.
A.7 Determination of hydrochloric acid insoluble matter
A.7.1 Methodological Summary
The sample is dissolved in hydrochloric acid, filtered with a glass sand core funnel, washed, dried, weighed, calculated insoluble content.
A.7.2 Reagents and materials
A.7.2.1 hydrochloric acid solution (1 1, volume ratio).
A.7.2.2 Glass sand core funnel.
A.7.3 Analysis steps
Weigh 5g sample (accurate to 0.001g), add hydrochloric acid solution (A.7.2.1) 10mL and water 50mL, mixed and heated for 30min,
Solution into the glass sand core funnel filter, vacuum pump suction filter, with.200mL water 5 times after washing the precipitate, the glass sand core funnel with the sediment
Drying in the oven at 105 ℃ for 2h, cooling, weighing, so many times repeated until constant weight.
A.7.4 Calculation of results
The mass fraction w3 of the hydrochloric acid insoluble matter is calculated according to formula (A.4)
w3 =
m2-m1
m x 100%
(A.4)
Where.
m1 --- the quality of the glass sand core funnel, in grams (g);
m2 --- glass sand core funnel and hydrochloric acid insoluble material quality, in grams (g);
m --- the quality of the sample, in grams (g).
The arithmetic mean of the parallel measurement results is the result of the measurement, and the difference between the two parallel measurements does not exceed 5% of the arithmetic mean.
A.8 Determination of solubility
A.8.1 Methodological Summary
The sample was dissolved in water, filtered through a glass sand core crucible, dried and weighed to calculate the content of insoluble matter, and the solubility index was obtained.
A.8.2 Reagents and Materials
A.8.2.1 Conical flask.
A.8.2.2 Glass sand core crucible.
A.8.3 Analysis steps
Weigh 0.45g sample (accurate to 0.001g) in a conical flask, add water 100mL, shake for 3min to dissolve, the solution into the glass
Sand crucible (crucible pre-drying weighing), filter, crucible with the precipitate at 105 ℃ drying 2h after cooling and weighing.
A.8.4 Calculation of results
Solubility M, calculated according to formula (A.5).
M = 1-
m2-m1
÷ × 100% (A.5)
Where.
m1 --- glass sand core crucible quality, unit grams (g);
m2 --- glass sand core crucible and insoluble material quality, in grams (g);
m --- the quality of the sample, in grams (g).
The arithmetic mean of the parallel measurement results is the result of the measurement, and the difference between the two parallel measurements does not exceed 5% of the arithmetic mean.
Appendix B
Citric acid malate calcium infrared spectrum
The infrared spectrum of calcium citrate malate is shown in Figure B.1.
Figure B.1 Infrared spectrum of calcium citrate malate
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