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GB 25555-2010: National food safety standards of food additives L-calcium lactate
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National food safety standards of food additives L-calcium lactate
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GB 25555-2010
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Basic data | Standard ID | GB 25555-2010 (GB25555-2010) | | Description (Translated English) | National food safety standards of food additives L-calcium lactate | | Sector / Industry | National Standard | | Classification of Chinese Standard | X40 | | Classification of International Standard | 67.220.20 | | Word Count Estimation | 13,166 | | Date of Issue | 2010-12-21 | | Date of Implementation | 2011-02-21 | | Regulation (derived from) | Ministry of Health Bulletin No. 19 of 2010 | | Issuing agency(ies) | Ministry of Health of the People's Republic of China | | Summary | This Chinese standard applies to fermentation production of L- lactic acid and calcium carbonate (or calcium hydroxide) synthesis system for food additives L- lactate. | GB 25555-2010: National food safety standards of food additives L-calcium lactate---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.
National food safety standards of food additives L-calcium lactate
National Standards of People's Republic of China
National standards for food safety
Food Additives L-Lactate
2010-12-21 release
2011-02-21 Implementation
Issued by the Ministry of Health of the People's Republic of China
Foreword
Appendix A of this standard is a normative appendix.
National standards for food safety
Food Additives L-Lactate
1 Scope
This standard is applicable to the production of L-lactic acid produced by fermentation and calcium carbonate (or calcium hydroxide) synthesis of food additives L-lactic acid calcium.
2 normative reference documents
The documents cited in this standard are indispensable for the application of this standard. Any reference to the date of the document, only the date of the edition
This applies to this standard. For undated references, the latest edition (including all amendments) applies to this standard.
3 Chemical name, molecular formula, structural formula and relative molecular mass
3.1 Chemical name
calcium α-hydroxypropionate
3.2 Molecular formula
C6H10CaO6 xH2O (x = 0 to 5)
3.3 Structural formula
3.4 Relative molecular mass
218.22 (anhydrous) (according to.2007 International relative atomic mass)
4 technical requirements
4.1 sensory requirements. should be consistent with the provisions of Table 1.
Table 1 sensory requirements
The project requires a test method
Color white
Smell no smell
Tissue state particles or powder
Take appropriate laboratory samples, placed in a clean, dry glass culture dish, in the natural light,
From the top and side to observe the color and appearance, smell the smell
4.2 Physical and chemical indicators. should be consistent with the provisions of Table 2.
Table 2 Physical and chemical indicators
Item Index Test Method
Stereochemical purity (L) /% ≥ 96.0 Appendix A A.4
Total Lactate (based on dry basis), w /% 98.0 to 101.0 Appendix A A.5
Dry reduction, w /%
22.0 ~ 27.0 (five water); 15.0 ~ 20.0 (Sanshui);
5.0 ~ 8.0 (a water); ≤ 3.0 (no water)
Appendix A, A.6
The water dissolution test was carried out in Test Appendix A, A.7
The free acid and free base tests were carried out in Test Appendix A, A.8
Volatile Fatty Acid Tests Tested in Appendix A, A.9
Magnesium and alkali metals, w /% ≤ 1.0 Appendix A. A.10
Chloride (in terms of Cl), w /% ≤ 0.05 Appendix A A.11
Sulfate (in SO4), w /% ≤ 0.075 Appendix A. A.12
Iron (Fe), w /% ≤ 0.005 Appendix A A.13
Arsenic (As)/(mg/kg) ≤ 2 Appendix A A.14
Lead (Pb)/(mg/kg) ≤ 2 Appendix A A.15
Barium (Ba) test through the test Appendix A A.16
Fluoride (in terms of F), w /% ≤ 0.0015 Appendix A A.17
Appendix A
(Normative appendix)
Testing method
A.1 Warning
Some of the test procedures specified in the test method may result in a hazardous situation. Operators should take appropriate safety and protective measures.
A.2 General provisions
Unless otherwise stated, only the reagents identified as analytical reagents and the tertiary water specified in GB/T 6682-2008 are used in the analysis.
Standard titration solution used in the test method, standard solution for the determination of impurities, preparations and articles, in the absence of other requirements,
GB/T 601, GB/T 602 and GB/T 603.
A.3 Identification test
A.3.1 Reagents and materials
A.3.1.1 Sulfuric acid.
A.3.1.2 Potassium permanganate solution. 3.2 g/L.
A.3.1.3 Ammonium oxalate solution. 40 g/L.
A.3.1.4 Hydrochloric acid solution. 1 3.
A.3.1.5 Acetic acid solution. 1 20.
A.3.2 Analysis steps
A.3.2.1 Identification of calcium salts
Take about 0.5g of laboratory samples, dissolved in 10mL water, dropping ammonium oxalate solution, which produces a white precipitate. Separate the precipitate and add acetic acid
Liquid, the precipitate does not dissolve; then add hydrochloric acid solution, the precipitate is completely dissolved.
A.3.2.2 Identification of lactate
Take about 0.5g laboratory samples, add 10mL of hot water dissolved, add sulfuric acid to make it acidic, add potassium permanganate solution, heating, that is issued
The smell of acetaldehyde.
A.4 Determination of stereochemical purity (L)
A.4.1 Methodological Summary
The L-lactate and D-lactic acid calcium group were determined by high performance liquid chromatography (HPLC) under the selected working conditions.
Fractional separation, detection with UV absorption detector, with the area normalization method to calculate the total Lactate calcium L calcium lactate content, that is, L-lactic acid
Stereochemical purity of calcium.
A.4.2 Reagents and materials
Copper sulfate solution. 0.001mol/L.
A.4.3 Instruments and equipment
A.4.3.1 High Performance Liquid Chromatography System (HPLC)
A.4.3.1.1 High pressure pump. no pulse, can keep the flow rate from 0.1mL/min ~ 10.0mL/min.
A.4.3.1.2 Dosing ring. 5 μL.
A.4.3.1.3 UV detector. Variable wavelength.
A.4.3.1.4 Data processing systems. Chromatographic workstations or data processors.
A.4.3.2 Filtration system
The filter system uses a cellulose ester membrane filter with a pore size of 0.45 μm (for pretreatment of the mobile phase).
A.4.3.3 Filtration systems
The filtration system uses a cellulose ester membrane filter with a pore size of 0.45 m (for pretreatment of the sample).
A.4.3.4 Micro injection needle
HPLC specific, 50 μL, 100 μL (or autosampler).
A.4.4 Chromatographic analysis conditions
The recommended columns and typical operating conditions are shown in Table A.1. Determination of Stereo Chemical Purity (L). Typical High Performance Liquid Chromatography
Figure A.1. Retention time. L-lactic acid calcium about 18.5min, D-lactic acid calcium about 23.5min (retention time will change to standard samples
Peak time). Other columns and chromatographic operating conditions that can achieve the same degree of separation can be used.
Table A.1 Columns and Typical Chromatographic Operating Conditions
Column
Column length 150mm, column diameter 4.6mm, with coordination exchange of optically active stationary phase coated with ODS dioxide
Silica packed chiral column
Column temperature 20 ℃ ~ 40 ℃, control accuracy ± 1 ℃
Mobile phase copper sulfate solution
Flow rate/(mL/min) 1.0
Detector detection wavelength/nm 254
Injection volume/μL 5 (injection of lactic acid concentration of about 0.1%), D body and L body separation of 1.0 or more
1 --- L body lactate;
2 --- D body calcium lactate.
Figure A.1 Stereochemical purity (L) determination of typical high performance liquid chromatography
A.4.5 Analysis steps
A.4.5.1 Sample preparation
Weigh the laboratory sample about 0.15g, accurate to 0.001g, heated water dissolved, transferred to 100mL volumetric flask, diluted to the mark,
Shaking back.
A.4.5.2 Determination
According to the instrument manual, adjust the instrument to the operating conditions shown in Table A.1, after the instrument is stable to start the determination. With microinjection
Or with an autosampler to sample, calculate the results with a chromatographic data processor or workstation, and quantify the area normalization method.
A.4.6 Calculation of results
Stereochemical purity (L) is the total content of calcium L-lactate in calcium lactate in the total lactate, and the value is expressed in%, calculated according to the formula (A.1)
X1 = AlAl Ad ×
100% (A.1)
Where.
Al - L peak concentration of calcium lactate component;
Ad - D concentration of calcium lactate component.
The arithmetic mean of the results of two parallel measurements is the result of the report. The absolute difference between the two parallel determinations is not more than 0.2%.
Determination of total calcium lactate (dry basis)
A.5.1 Methodological Summary
Under normal conditions, the total milk was calculated from the volume of the standard titrant of disodium ethylenediaminetetraacetic acid disodium
Calcium content of calcium, calcium reagent used to determine the color of sodium chloride indicator to determine the end point of titration.
A.5.2 Reagents and materials
A.5.2.1 Sodium hydroxide solution. 100 g/L.
A.5.2.2 Hydrochloric acid solution. 1 4.
A.5.2.3 Standard titration solution of disodium ethylenediamine tetraacetate. c (EDTA) = 0.05 mol/L.
A.5.2.4 calcium reagent sodium carboxylate indicator. Weigh 0.1g calcium reagent sodium carboxylate salt, add 10g of sodium chloride dried at about 110 ℃
Grinding, mixing.
A.5.3 Analysis steps
Weigh about 0.3g A.6.1 dry matter A, accurate to 0.0002g, dissolved in 2mL hydrochloric acid solution has been added in 50mL of water, side
Add 15mL ethylenediamine tetraacetic acid disodium standard titration solution, add 5mL sodium hydroxide solution and 0.1g calcium reagent sodium carboxylate
Indicator, with ethylenediamine tetraacetic acid disodium standard titration solution to the solution showed blue as the end point.
A.5.4 Calculation of results
The mass fraction of total calcium lactate, w2, is expressed in%, calculated according to formula (A.2)
w2 =
(V/1000) cM
m x 100%
(A.2)
Where.
V --- sample consumption of ethylenediamine tetraacetic acid disodium standard titration solution volume value in milliliters (mL);
c - Ethylenediamine tetraacetic acid disodium standard titration solution concentration of the exact value in moles per liter (mol/L);
m - the mass of the sample, in grams (g);
M - Calcium lactate (C6H10CaO6), in grams per mole (g/mol) (M = 218.2).
The arithmetic mean of the results of two parallel measurements is the result of the measurement. The absolute difference between the two parallel determinations is not more than 0.2%.
A.6 Determination of dry reduction
A.6.1 Analysis steps
Weigh about 1.5g of laboratory samples, accurate to 0.0002g, placed in the (120 ± 2) ℃ dry to the constant quality of the flat weighing
Bottle, paved 3mm below the layer. In the (120 ± 2) ℃ constant temperature drying oven for 4h, placed in a dryer for 30min cooling.
A portion of the dried product (this is dry matter A) is used for the determination of total calcium lactate content.
A.6.2 Calculation of results
The mass fraction of dry weight w3, expressed in%, is calculated according to formula (A.3).
w3 = m-m1m x 100%
(A.3)
Where.
m - the mass of the sample before drying, in grams (g);
m1 --- the quality of the sample after drying, in grams (g).
The arithmetic mean of the results of two parallel measurements is the result of the report. The absolute difference between the two parallel determinations is not more than 0.2%.
A.7 Water Dissolution Test
A.7.1 Reagents and materials
A.7.1.1 Nitric acid solution. 1 2.
A.7.1.2 Dextrin solution. 20 g/L.
A.7.1.3 Silver nitrate solution. 17 g/L.
A.7.1.4 Turbidity standard solution. chlorine (Cl) 0.01mg/mL. The amount of c (HCl) = 0.1mol/L hydrochloric acid standard solution 14.1mL,
Placed in 50mL volumetric flask, diluted with water to the mark. Measure the solution 10.00mL, placed in a 1000mL volumetric flask, diluted with water
Scale.
A.7.2 Analysis steps
Weigh 1.0g of laboratory samples, accurate to 0.01g, placed in 25mL colorimetric tube, add 20mL of water, dissolved in the water bath,
As the test solution; take another color tube, add (0.20 ± 0.02) mL turbidity standard solution, add water to 20mL, add 1mL nitric acid solution,
0.2mL dextrin solution and 1mL silver nitrate solution, shake, dark place 15min, as the standard turbid solution. In the absence of direct sunlight
, The turbidity of the test solution shall not be greater than the turbidity of the standard turbid solution.
A.8 Free acid and free base test
A.8.1 Reagents and materials
A.8.1.1 sodium hydroxide standard solution. c (NaOH) = 0.1mol/L.
A.8.1.2 phenolphthalein indicator solution. 10g/L.
A.8.2 Analysis steps
Weigh 1.0g of laboratory samples, accurate to 0.01g, dissolved in 20mL of carbon dioxide without water, add 3 drops of phenolphthalein indicator solution, should not have powder
Red generation; plus 0.5mL sodium hydroxide standard solution, should be pink.
A.9 Volatile Fatty Acid Test
Weigh about 0.5g of laboratory samples, accurate to 0.01g, placed in a dry evaporative dish, add 1mL of sulfuric acid, stir, heated in the water bath,
There should be no smell of fatty acids.
Determination of magnesium and alkali metal content
A.10.1 Methodological Summary
Calcium in the sample under acidic conditions and oxalic acid to produce insoluble calcium oxalate precipitation, filtration, the filtrate of magnesium and alkali metal and sulfuric acid heating students
Into the sulfate, and then filter, the filtrate evaporated, quantitative after burning.
A.10.2 Reagents and materials
A.10.2.1 Hydrochloric acid.
A.10.2.2 Sulfuric acid.
A.10.2.3 Ammonia.
A.10.2.4 oxalic acid solution. 150 g/L.
A.10.2.5 methyl red indicator solution. 1g/L.
A.10.3 Analysis steps
Weigh 1.0g of laboratory samples, accurate to 0.01g, add water 40mL, plus 1mL hydrochloric acid, boil 1min, quickly add 40mL grass
Acid solution and 2 drops of methyl red indicator solution, neutralized with ammonia to the solution just yellow, cooled to room temperature. Into the 100mL volumetric flask, dilute
Release to scale, shake, place for 4h or overnight. Filtration with dry filter paper, take 50mL clear filtrate, placed in advance (800 ± 25) ℃ drying
To the constant quality of the crucible, add 0.5mL sulfuric acid, in the water bath evaporated to near dry, heated in the electric furnace to the sulfuric acid vapor escape, in the (800 ±
25) ℃ to a constant mass. Residue quality should not be greater than 5.0mg.
A.11 Determination of Chloride
According to the "People's Republic of China Pharmacopoeia".2005 edition of the two Appendix Ⅷ A regulations. Weigh 0.1g of laboratory samples, accurate to
0.001g, its turbidity should not be greater than the standard turbid solution. (5 ± 0.02) mL of chloride (Cl) standard solution (0.01 mg/mL)
Preparation of standard turbid solution.
A.12 Determination of sulfate
According to the "People's Republic of China Pharmacopoeia".2005 edition of the two Appendix Ⅷ B regulations. Weigh the sample 0.20g, accurate to 0.001g,
Its turbidity shall not be greater than the standard turbid solution. (1.5 ± 0.02) mL of sulfate (SO4) standard solution (0.1 mg/mL)
Standard turbid solution.
A.13 Determination of iron
According to the "People's Republic of China Pharmacopoeia".2005 edition of the two Appendix Ⅷ G regulations. Weigh 0.5g laboratory samples, accurate to
0.01g, add 25mL water, placed in a water bath to dissolve, after cooling for the test solution, its color should not be deeper than the standard colorimetric solution.
A standard colorimetric solution was prepared by measuring (2.5 ± 0.02) mL of iron (Fe) standard solution (0.01 mg/mL).
A.14 Determination of arsenic
According to GB/T 5009.76 arsenic spot method. Determination of 1.0g laboratory samples, accurate to 0.01g, add 10mL of hot water
Dissolve.
Preparation of the standard solution. 2.00mL arsenic (As) standard solution (equivalent to 0.002mgAs) was removed from the pipette,
The same treatment.
A.15 Determination of lead
According to GB/T 5009.75 "limited test". Sample treatment. Weigh 3.0g sample, accurate to 0.01g, heated water 30mL
Dissolved, into the separatory funnel, add 1% nitric acid to 40mL. Measure the amount of 0.60 mL lead (Pb) standard solution (equivalent to 0.006 mgPb)
Prepaid Lead Standard.
A.16 barium test
Weigh 1.0g of laboratory samples, accurate to 0.01g, add 20mL of hot water dissolved, divided into two equal parts placed in two 25mL colorimetric tube
, A plus 1mL calcium sulfate saturated solution mix, another plus 1mL water, after 15min after the comparison, the sample tube was not large
In the control tube.
A.17 Determination of fluoride
A.17.1 Methodological Summary
In the perchloric acid medium, the fluorine is separated from the sample by steam distillation, and the mixture of fluorine and alizarin ammonia complexing agent and lanthanum nitrate forms blue
Color complex, measured at 620nm its absorbance, according to the working curve to calculate the fluoride content of the sample.
A.17.2 Reagents and materials
A.17.2.1 Acetone.
A.17.2.2 perchloric acid.
A.17.2.3 Sodium hydroxide solution. 4 g/L.
A.17.2.4 Sodium hydroxide solution. 40 g/L.
A.17.2.5 Silver nitrate solution. 2 g/100 mL.
A.17.2.6 Hydrochloric acid. 1 10.
A.17.2.7 Lanthanum nitrate solution. Weigh 0.22 g of lanthanum nitrate, dissolve with a small amount of acetic acid solution (3 47), add water to about 450 mL,
Sodium solution (250g/L) to adjust the pH to 5.0, then diluted with water to 500mL, set the refrigerator (6 ℃ ~ 8 ℃) preservation, mildew after re-allocation.
A.17.2.8 Buffer (pH 4.7). Weigh 44g of sodium acetate, dissolve in 400 mL of water, add 22 mL of glacial acetic acid, then slowly add glacial acetic acid
Adjust the pH to 4.7, then add water to 500mL.
A.17.2.9 Fluorine standard solution. 0.01 mg/mL.
Weigh 0.215g of sodium fluoride dried at 105 ℃ for 2h, and accurate to 0.0002g. Dissolved in water, into the 100mL volumetric flask, add water
To the scale, mix, stored in the polyethylene bottle in reserve, set the refrigerator to save, the fluorine standard stock solution concentration of 1.0mg/mL.
Before use, draw (1 ± 0.02) mL of fluorine standard stock solution, diluted to 100mL, mix, stored in the polyethylene bottle. This is
0.01 mg/mL of fluorine standard solution.
A.17.2.10 phenolphthalein indicator solution. 10g/L.
A.17.2.11 alizarin ammonia complexing agent solution. Weigh 0.193g alizarin ammonia complexing agent, add a small amount of water and sodium hydroxide solution (40g/L)
Dissolve it, add 0.13 g of sodium acetate, adjust the pH to 5.0 (red) with 1 mol/L acetic acid, dilute to 500 mL with water, and store in a brown
In the refrigerator (6 ℃ ~ 8 ℃) to save, should be re-prepared precipitation.
A.17.3 Instruments and equipment
A.17.3.1 Spectrophotometer. A quartz cuvette with an optical path length of 30 mm with an absorbance accuracy of ± 0.004 (A).
A.17.3.2 Schematic diagram of the fluorinated distillation unit is shown in Figure A.2.
1 --- water vapor generator (1000mL flask);
2 --- rubber stopper;
3 --- φ5mm glass tube;
4 --- tee and screw clip;
5 ---.200 ℃ thermometer;
6 --- 250mL three-necked flask;
7 --- heating sleeve or electric furnace;
8 --- glass elbow;
9 --- 500mm straight condenser;
10 --- 250mL volumetric flask.
Figure A.2 Schematic diagram of a fluorinated distillation unit
A.17.4 Analysis steps
A.17.4.1 Drawing of Fluorine Standard Curves
Respectively, draw 0mL, 0.5mL, 1.0mL, 1.5mL, 2.0mL, 2.5mL fluoride standard solution placed in 6 50mL colorimetric
(5 ± 0.02) mL of alizarin ammonia complexing solution and (3 ± 0.02) mL of buffer were added to each colorimeter and mixed. Slowly add (5 ±
0.02) mL of lanthanum nitrate solution, shake, add (10 ± 0.02) mL of acetone, add water to 50mL, mix, room temperature for 25min. Move in
30mm quartz cuvette, measured at a wavelength of 620nm absorbance; with fluoride mass as the abscissa, the corresponding absorbance for the vertical axis, painted
Standard curve.
A.17.4.2 Determination
Weigh 2g laboratory samples, accurate to 0.01g, placed in 250mL three-necked flask, add glass beads 5 to 6, slowly adding perchloric acid
10mL, with about 8mL of water rinse the wall, add silver nitrate test solution 4 to 6 drops; according to the fluorine distillation device schematic diagram (see Figure A.2) connected to the device,
The thermometer should be inserted into the test solution, and the glass elbow at the end of the condenser is inserted into the test solution.
90 mL of sodium hydroxide solution (A.17.2.3) and 2 drops of phenolphthalein in a 250 mL volumetric flask. Water vapor generator by adding 500mL of water,
5 to 10 pieces of glass beads; and dropping sodium hydroxide solution (A.17.2.4) to make alkaline. Open the screw clip and heat it to near boiling. Close the screw clip,
The water vapor was passed through a 250 mL three-necked flask while the three-necked flask was heated to adjust the amount of water vapor to keep the temperature
135 ° C to 140 ° C; if the solution in the volumetric flask fades, add the appropriate amount of sodium hydroxide solution (A.17.2.3), keep the distillate into the base
, Until.200 mL, to stop the distillation; with sodium hydroxide solution (A.17.2.3) and hydrochloric acid solution to adjust the pH is neutral (with precision pH test paper
Test), plus hydrochloric acid solution 2 drops, add water to 250mL, shake, as the test solution. Extract (25 ± 0.02) mL of sample from the volumetric flask
(5 ± 0.02) mL of alizarin ammonia complexing solution and (3 ± 0.02) mL of buffer in the colorimetric tube. Slowly add (5 ±
0.02) mL of lanthanum nitrate solution, shake, add (10 ± 0.02) mL of acetone, add water to 50mL, mix, room temperature for 25min. Move in
30 mm quartz cuvette, absorbance was measured at a wavelength of 620 nm. The quality of the fluorine is determined according to the pre-determined standard curve.
A.17.5 Calculation of results
The mass fraction w4 of the fluoride (in terms of F), expressed in%, is calculated according to the formula (A.4)
w4 = 10m11000m × 100%
(A.4)
Where.
m1 - the mass of fluorine injected into the spectrophotometer sample in milligrams (mg);
m --- the quality of the sample, in grams (g).
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