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GB 25544-2010: DL-malic acid of the national food safety standards of food additives
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DL-malic acid of the national food safety standards of food additives
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GB 25544-2010
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Basic data | Standard ID | GB 25544-2010 (GB25544-2010) | | Description (Translated English) | DL-malic acid of the national food safety standards of food additives | | Sector / Industry | National Standard | | Classification of Chinese Standard | X42 | | Classification of International Standard | 67.220.20 | | Word Count Estimation | 12,137 | | 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 maleic anhydride, cis/fumaric acid as raw material by hydration, concentration crystallization, dehydration, drying and prepared food additives DL- malic acid. | GB 25544-2010: DL-malic acid of the national food safety standards of food additives---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.
DL-malic acid of the national food safety standards of food additives
National Standards of People's Republic of China
National standards for food safety
Food additives DL-malic acid
2010-12-21 release
2011-02-21 Implementation
Issued by the Ministry of Health of the People's Republic of China
Foreword
Appendix A, Appendix B and Appendix C of this standard are normative appendices.
National standards for food safety
Food additives DL-malic acid
1 Scope
This standard is suitable for the use of maleic anhydride, cis/fumaric acid as raw materials by hydration reaction, concentrated crystallization, dehydration, drying and prepared
Food additives DL-malic acid.
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
DL-hydroxy succinic acid
3.2 Molecular formula
C4H6O5
3.3 Structural formula
HO CH COOH
CH2 COOH
3.4 Relative molecular mass
134.09 (according to.2007 International Relative Atomic Quality)
4 technical requirements
4.1 sensory requirements. should be consistent with the provisions of Table 1.
Table 1 sensory requirements
Item Index Test Method
Color white or white
Odor has a special sour taste
Organizational state Crystallization powder or granules
Take appropriate laboratory samples and place them in a clean, dry white porcelain dish
In the natural light, visual observation, 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
DL-malic acid (based on C4H6O5), w /% 99.0 to 100.5 Appendix A, A.4
Specific rotation αm (25 ℃, D)/[(°) · dm2 · kg-1] -0.10 ~ 0.10 Appendix A A.5
Arsenic (As)/(mg/kg) ≤ 2 Appendix A A.6
Lead (Pb)/(mg/kg) ≤ 2 Appendix A A.7
Residue on ignition, w /% ≤ 0.1 Appendix A A.8
Fumaric acid, w /% ≤ 1.0 Appendix A A.9
Maleic acid, w /% ≤ 0.05 Appendix A A.9
Water insoluble matter, w /% ≤ 0.1 A. A in Appendix A.
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 Malate Ammonia Salt coloring test
A.3.1.1 Reagents and materials
A.3.1.1.1 Ammonia solution. 2 3.
A.3.1.1.2 p-aminobenzenesulfonic acid. 10 g/L.
A.3.1.1.3 Sodium nitrite solution..200 g/L.
A.3.1.1.4 Sodium hydroxide solution. 40 g/L.
A.3.1.2 Analysis steps
Weigh 0.5g of laboratory samples, accurate to 0.01g, placed in 50mL test tube, add 10mL of water dissolved. Neutralized with aqueous ammonia solution
To neutral, add 1mL p-aminobenzenesulfonic acid solution and heat in a boiling water bath for 5min. Add 5mL sodium nitrite solution, and then placed in a water bath
After heating for 3 min, add 5 mL of sodium hydroxide solution, the test solution should be red immediately.
A.3.2 Infrared Spectrum Control
Weigh about 1mg of laboratory samples and 100mg potassium bromide, research into uniform powder, into the former, after pressing into the film with infrared
The spectra of the DL-malic acid are shown in Figure B.1, and the spectra are consistent with the DL-malic acid standard.
A.4 Determination of DL-malic acid content
A.4.1 Methodological Summary
The aqueous solution of the sample was titrated with the standard solution of sodium hydroxide with phenolphthalein as the indicator, and the amount of the solution was titrated according to the standard of sodium hydroxide.
The total acid content of C4H6O5 is DL-malic acid content.
A.4.2 Reagents and materials
A.4.2.1 sodium hydroxide standard sodium titration solution. c (NaOH) = 1.0mol/L.
A.4.2.2 phenolphthalein indicator solution. 10g/L.
A.4.3 Analysis steps
A.4.3.1 Weigh 2.0g of laboratory samples, accurate to 0.0002g, add 40mL of water without carbon dioxide dissolved, add 2 drops of phenolphthalein instructions
Liquid, titration with sodium hydroxide standard solution to reddish, keep 30s do not fade for the end.
A.4.3.2 At the same time as the determination, the same amount of reagent solution was used as a blank test in the same procedure as for the measurement.
A.4.4 Calculation of results
DL-malic acid (based on C4H6O5), the value is expressed in%, calculated according to the formula (A.1)
w1 =
[(V-V0)/1000] cM
m x 100%
(A.1)
Where.
V --- sample consumption of sodium hydroxide standard titration solution (A.4.2.1) volume of the value in milliliters (mL);
V0 --- blank test consumption of sodium hydroxide standard titration solution (A.4.2.1) volume of the value in milliliters (mL);
c - the exact value of sodium hydroxide standard titration solution concentration in moles per liter (mol/L);
m - the mass of the sample, in grams (g);
M - malic acid (1/2C4H6O5) in grams per mole (g/mol) (M = 67.04).
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.5 Determination of specific rotation
A.5.1 Weigh 4.25 g of laboratory sample, accurate to 0.001g, add 20mL of water to dissolve, move to 50mL volumetric flask, diluted with water
To the scale, shake. The measurement temperature was 25 ° C ± 0.5 ° C.
The value of the specific rotation αm (25 ° C, D) is expressed by (°) · dm2 · kg-1, calculated according to the formula (A.2)
αm (25 ° C, D) = α lρα
(A.2)
Where.
α - the measured angle of rotation, in degrees (°);
l - the length of the rotating tube in dm (dm);
ρα - Mass concentration of the effective components in solution, in grams per milliliter (g/mL).
A.5.2 Other according to GB/T 613.
A.6 Determination of arsenic
A.6.1 Weigh 1.0g of laboratory samples, accurate to 0.01g, into the arsenic device into the conical flask, add 5mL of water dissolved, add 1 drop
Bromophenol blue indicator solution (0.4g/L), dropping ammonia solution (14) and the solution was purple, replenishment to about 35mL, then add 20mL sulfur
Acid solution (1 5), shake, as the sample solution. Use Absorbent Solution B. Perform a limited test to measure 2 mL ± 0.02 mL arsenic (As) standard
Solution (equivalent to 2.0 μgAs) to prepare a limited standard solution.
A.6.2 other according to GB/T 5009.76 diethylamino dithiocarbamate colorimetric method.
A.7 Determination of lead
A.7.1 Colorimetric method (Arbitration law)
According to GB/T 5009.75. The sample treatment was carried out by dry digestion. Before use, 1mg/mL lead (Pb) standard solution dilute
Release 5 μg/mL lead (Pb) standard solution. Measure 25mL ± 0.02mL sample solution (equivalent to 2.5g laboratory samples
) And 1 mL of ± 0.02 mL lead (Pb) standard solution (equivalent to 5 μg of Pb) were placed in a 125 mL separatory funnel and the lead standard solution
Add 1% nitric acid solution to 25mL.
A.7.2 Atomic Absorption Spectrometry
Specimen treatment according to GB/T 5009.75 dry digestion method. Others are carried out according to GB 5009.12.
A.8 Determination of burning residue
Weigh about 2g of laboratory samples, accurate to 0.0001g. The burning temperature is 800 ° C ± 25 ° C. Other according to GB/T 9741.
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 0.01%.
A.9 Determination of fumaric acid and maleic acid
A.9.1 Methodological summary
The components of the sample solution were separated by high performance liquid chromatography under the selected working conditions, and the samples were separated by UV absorption
The content of fumaric acid and maleic acid in the sample was calculated by external standard method.
A.9.2 Reagents and materials
A.9.2.1 Fumaric acid. mass fraction ≥99.0%.
A.9.2.2 Maleic acid. mass fraction ≥99.0%.
A.9.2.3 Sodium hydroxide solution. 20 g/L.
A.9.2.4 phosphoric acid solution. the amount of phosphoric acid (excellent grade) 1mL ± 0.02mL in 1000mL volumetric flask, add 100mL methanol
(HPLC grade, according to the column to adjust the amount of added), diluted with water to the mark, and then filtered through the 0.45μm filter.
A.9.3 Instruments and equipment
A.9.3.1 High Performance Liquid Chromatography System (HPLC)
A.9.3.1.1 High pressure pump. no pulse, can keep the flow rate from 0.1mL/min ~ 10.0mL/min.
A.9.3.1.2 Dosing ring. 5 μL.
A.9.3.1.3 UV detector. variable wavelength.
A.9.3.1.4 Data processing systems. Chromatographic workstations or data processors.
A.9.3.2 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.9.3.3 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.9.3.4 injector
Autosampler or microinjector, 50 [mu] L or 100 [mu] L.
A.9.4 Chromatographic analysis conditions
Recommended column and typical chromatographic operating conditions are given in Table A.1. Fumaric acid and maleic acid assays Typical high performance liquid chromatograms are given in Appendix C
Figure C.1, the relative retention time of each component is given in Appendix C, Table C.1. Other columns that can achieve the same degree of separation and chromatographic operating conditions
Can be used.
Table A.1 Columns and Typical Chromatographic Operating Conditions
Column column length 250mm, column diameter 4.6mm, silica gel as the matrix, the surface bonding C8 functional non-polar packing column
Column temperature 15 ℃ ~ 60 ℃, control accuracy ± 1 ℃
Mobile phase phosphoric acid solution
Flow rate/(mL/min) 1.0
Detector detection wavelength/nm 214
Injection volume/μL 5
A.9.5 Analysis steps
A.9.5.1 Preparation of standard sample solutions
A.9.5.1.1 Preparation of fumaric acid standard sample solution
Weigh 50mg fumaric acid, accurate to 0.0002g, dissolved in water (if necessary, add a small amount of sodium hydroxide solution), transferred to 50mL
Volumetric flask, diluted with phosphoric acid solution to the scale.
Remove the solution 1mL ± 0.02mL, placed in 50mL volumetric flask, diluted with phosphoric acid solution to the mark, shake, by 0.45μm filter
Membrane filtration, and then by ultrasonic degassing treatment.
A.9.5.1.2 Preparation of standard solution of maleic acid
Weigh 50mg maleic acid, accurate to 0.0002g, dissolved in the amount of water (if necessary, add a small amount of sodium hydroxide solution), transferred to
250mL volumetric flask, diluted with phosphoric acid solution to the scale.
Remove the solution 1mL ± 0.02mL, placed in 100mL volumetric flask, diluted with phosphoric acid solution to the mark, shake, by 0.45μm
Filter filter, and then by ultrasonic degassing treatment.
A.9.5.2 Preparation of sample solution
Weigh 0.2g of laboratory samples, accurate to 0.0002g, placed in 50mL volumetric flask, the mobile phase diluted to the mark, shake, by
0.45μm filter filter, and then by ultrasonic degassing treatment.
A.9.5.3 Determination
According to high-performance liquid chromatography operating procedures to start preheating, adjust the temperature and flow to achieve the conditions of analysis and baseline stable, the standard sample dissolved
Liquid injection.
5 μL of the standard sample solution was taken with a micro-injector, and the resulting fumaric acid or maleic acid peak was recorded by injection (or autosampling)
Product A2.
5 μL of the sample solution was sampled in a micro-injector, and the peak area A1 of the obtained substance was recorded by injection (or autosampling).
A.9.6 Calculation of results
Fumaric acid or maleic acid mass fraction w2, expressed in%, calculated according to formula (A.3).
w2 = A1 × m2A2 × m ×
100% (A.3)
Where.
A1 --- peak area of the substance to be tested in the sample solution;
A2 - peak area of fumaric acid or maleic acid in standard sample solution;
m2 --- the amount of fumaric acid or maleic acid in the standard sample solution in micrograms (μg);
m - the amount of sample injected in micrograms (μg).
A.10 Determination of water insoluble matter
A.10.1 Analysis steps
Weigh 25.0 g of laboratory samples, accurate to 0.1g, dissolved in 100mL water to dry to a constant crucible acid filter leak
After the filter was filtered, the funnel was washed with hot water and dried in a 100 ° C oven to constant weight and cooled and weighed.
A.10.2 Calculation of results
The mass fraction of water insoluble matter w3, expressed in%, is calculated according to equation (A.4).
w3 = m1m x 100%
(A.4)
Where.
m1 --- the value of the quality of residue, in grams (g);
m - the mass of the sample, in grams (g).
Appendix B
(Normative appendix)
DL-Malic Acid Infrared Standard Spectrum
Figure B.1 shows the DL-malic acid infrared standard spectra.
Figure B.1 DL-Malic Acid Infrared Standard Spectrum
Appendix C.
(Normative appendix)
Fumaric acid and maleic acid were used to determine the typical high performance liquid chromatograms and the relative retention times of the components
C.1 Figure C.1 shows a typical high performance liquid chromatogram for fumaric acid and maleic acid.
1 --- DL-malic acid;
2 --- maleic acid;
3 --- fumaric acid.
Figure C.1 Typical high performance liquid chromatography for fumaric acid and maleic acid determination
C.2 Table C.1 shows the relative retention times for each component.
Table C.1 Relative Retention Time for Each Component
Peak sequence name relative retention time
1 DL-malic acid 1
2 maleic acid 1.34
3 fumaric acid 1.74
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