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GB 13737-2008: Food additive -- L-Malic acid
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PDF similar to GB 13737-2008
Basic data | Standard ID | GB 13737-2008 (GB13737-2008) | | Description (Translated English) | Food additive -- L-Malic acid | | Sector / Industry | National Standard | | Classification of Chinese Standard | X42 | | Classification of International Standard | 67.220.20 | | Word Count Estimation | 11,141 | | Date of Issue | 2008-06-25 | | Date of Implementation | 2009-01-01 | | Older Standard (superseded by this standard) | GB 13737-1992 | | Quoted Standard | GB/T 601-2002; GB/T 602-2002; GB/T 603-2002; GB/T 613-2007; GB/T 1250; GB/T 5009.12-2003; GB/T 5009.75-2003; GB/T 5009.76-2003; GB/T 6678; GB/T 6679; GB/T 6682-2008; GB/T 9729-2007; GB/T 9741-1988 | | Regulation (derived from) | Announcement of Newly Approved National Standards No. 12 of 2008 (No. 125 overall) | | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China | | Summary | This Chinese standard specifies the food additive L-malic acid requirements, test methods, inspection rules and signs, packaging, transportation and storage. This standard applies to the method of enzyme engineering, fermentation method were food additives L-malic acid. The product is mainly used as food acidity regulator. | GB 13737-2008: Food additive -- L-Malic acid---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 additive.L-Malic acid
ICS 67.220.20
X42
National Standards of People's Republic of China
Replacing GB 13737-1992
Food additives L- malic acid
Posted 2008-06-25
2009-01-01 implementation
Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
Standardization Administration of China released
Foreword
Chapter 5 and 8.1 of this standard are mandatory, the rest are recommended.
This standard replaces GB 13737-1992 "Food Additive L- malic acid."
This standard compared with GB 13737-1992, the main changes are as follows.
--- Increased the lead content item and the corresponding test methods (see Chapter 5 and 6.10);
--- Increasing the content of fumaric acid, maleic acid content of the project and the corresponding test methods (see Chapter 5 and 6.13);
--- Yi canceled oxide project and the appropriate test method (version 3.2 and 4.10 of 1992);
--- Sulfate content ≤0.03% by the index changed to ≤0.02%, chloride content index from the ≤0.005% revised to ≤0.004%,
Heavy metal content index from the ≤0.002% revised to ≤10mg/kg (1992 version 3.2, Chapter 5 of this edition);
--- L- malic acid content of measuring the concentration of sodium hydroxide solution by titration standard Huai 0.1mol/L adjusted to 1.0mol/L, and increase
The sample size (1992 version 4.4, this version 6.4);
--- Modify the sulfate determination (1992 version 4.5, this version 6.6);
--- Shelf life from one year to 24 months to modify (the 1992 version 6.4, this version 8.4).
Appendix A of this standard is an informative annex.
The standard proposed by China Petroleum and Chemical Industry Association.
This standard by the National Standardization Technical Committee branch of organic chemistry (SAC/TC63/SC2) and the National Food Additives Standardization
Committee (SAC/TC11) centralized.
This standard was drafted. Changmao Biochemical Engineering Company Limited.
Participated in the drafting of this standard. Biological Engineering Co., Ltd. Nanjing China Sea.
The main drafters of this standard. Rui Liqin, Zhupei Yun, Gong Xiaoyu.
This standard was first released in November 1992.
Food additives L- malic acid
1 Scope
This standard specifies the requirements for food additives L- malic acid, test methods, inspection rules and signs, packaging, transportation and storage.
This standard applies to enzyme engineering methods, obtained by fermentation of food additives L- malic acid. The products are mainly used for food acidity tune
Modifiers.
2 Normative references
The following documents contain provisions which, through reference in this standard, constitute provisions of this standard. For dated references, subsequent
Amendments (not including errata content) or revisions do not apply to this standard, however, encourage the parties to the agreement are based on research
Whether the latest versions of these documents. For undated reference documents, the latest versions apply to this standard.
Preparation of GB/T 601-2002 Chemical Reagent standard titration solution
GB/T 602-2002 Chemical Reagent preparation impurity standard solution measurement (ISO 6353-1. 1982, NEQ)
GB/T 603-2002 Chemical Reagent Test Methods Preparations with (ISO 6353-1. 1982, NEQ)
GB/T 613-2007 General method for determination of chemical reagents specific rotation ability (specific optical rotation)
Representation GB/T 1250 limit values and the method of determining
Determination of GB/T 5009.12-2003 lead in food
Determination of GB/T 5009.75-2003 food additives lead
Determination of GB/T 5009.76-2003 arsenic in food additives
GB/T 6678 General Principles for Sampling Chemical Products
GB/T 6679 General rules for sampling solid chemical products
GB/T 6682-2008 analytical laboratory use specifications and test methods (ISO 3696. 1987, MOD)
GB/T 9729-2007 General method for determination of chloride Chemicals
GB/T 9741-1988 Chemicals general method determination of residue on ignition
3 chemical name, molecular formula, molecular mass and structural formula
Chemical Name. L- malic acid
Molecular formula. C4H6O5
Structural Formula. HO CH
CH
2COOH
COOH
Molecular weight. 134.09 (according to 2007 international relative atomic mass)
4 Characters
White crystal or crystalline powder with special sour.
5 Requirements
L- malic acid food additives shall comply with the technical requirements in Table 1 below.
Table 1 Technical Requirements
Item Index
L- malic acid (C4H6O5 dollars), /% ≥ 99.0
Specific rotation αm (20 ℃, D)/[(°) · dm2 · kg-1] -1.6 ~ -2.6
Sulfate (SO4 dollars), /% ≤ 0.02
Chloride (Cl dollars), /% ≤ 0.004
Arsenic (As),/(mg/kg) ≤ 2
Heavy metals (Pb),/(mg/kg) ≤ 10
Lead (Pb),/(mg/kg) ≤ 2
Residue on ignition, /% ≤ 0.10
Clarity test by testing
Fumaric acid, /% ≤ 0.5
Maleic acid, /% ≤ 0.05
6 Test methods
6.1 Warning
Some test procedures prescribed test method can lead to dangerous situations. The operator shall take appropriate safety and health practices.
6.2 General Provisions
Unless otherwise indicated in the analysis using only confirm three analytical grade reagents and water GB/T 6682-2008 stipulated.
The test method used in the standard titration solution, impurities measured by standard solution, preparations and products, not specified in other requirements, according
GB/T 601-2002, regulations preparation GB/T 602-2002 and GB/T 603-2002 in.
6.3 Identification Test
6.3.1 malic acid ammonium salt colorimetric test
6.3.1.1 Reagents
6.3.1.1.1 ammonia solution. 2 + 3;
6.3.1.1.2 amino acid. 10g/L;
6.3.1.1.3 sodium nitrite solution.200g/L;
6.3.1.1.4 sodium hydroxide solution. 40g/L.
6.3.1.2 analysis step
Weigh 0.5g laboratory samples, accurate to 0.01g, placed in 50mL test tube, add water to dissolve 10mL. With aqueous ammonia solution
To neutral, the solution was added 1mL sulfanilic acid, heated in a boiling water bath for 5min. 5mL was added sodium nitrite solution, and then placed in a water bath
After heating 3min, was added 5mL sodium hydroxide solution, the test solution should be immediately red.
6.3.2 Optical characteristics test
Test methods with 6.5, the sample solution should feature was left-handed.
6.4 L- malic acid determination
6.4.1 Principle of the method
Phenolphthalein as indicator, titrated with sodium hydroxide aqueous solution standard sample, according to the amount of sodium hydroxide standard titration solution, calculated
In total acid C4H6O5 count for L- malic acid content.
6.4.2 Reagents
6.4.2.1 sodium hydroxide standard titration solution. Ba (NaOH) = 1.0mol/L;
6.4.2.2 phenolphthalein indicator solution. 10g/L.
6.4.3 Analysis of step
6.4.3.1 Weigh 2.0g laboratory samples, accurate to 0.0002g, add 20mL no carbon dioxide dissolved in water, add 2 drops of phenolphthalein indicator
Washed with sodium hydroxide standard solution titration to reddish, maintaining 30s does not fade as the end point.
6.4.3.2 measured at the same time, according to the same procedure and the determination of the sample without using the same amount of reagent blank test solution.
6.4.4 Calculation Results
L- malic acid (C4H6O5 meter) mass fraction of 1% to the value expressed by the formula (1).
1 =
[(Vp - V0)/1000] Ba M
(1)
Where.
Vp --- sample consumption of sodium hydroxide standard titration solution (6.4.2.1) the value of the volume, in milliliters (mL);
V0 --- consumption of sodium hydroxide standard titration blank test solution (6.4.2.1) the value of the volume, in milliliters (mL);
Accurate Ba --- sodium hydroxide standard titration solution concentration value in units of moles per liter (mol/L);
M --- (malic acid 12C4H6O) numerical molar mass of 5 units of grams per mole (g/mol) (M = 67.04).
Calculation result to two decimal places.
Take two parallel determination results of the arithmetic average of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.2%.
6.5 Determination of specific rotation
6.5.1 Weigh 4.25g laboratory samples, accurate to 0.001g, added 20mL of water to dissolve, move 50mL volumetric flask, diluted with water
To the mark.
Specific rotation αm (20 ℃, D) to the value "(°) · dm2 · kg-1" said, according to the formula (2).
(2)
Where.
α --- measured rotation angle in degrees (°);
Ρα --- mass concentration of the effective component in solution, in grams per milliliter (g/mL).
6.5.2 Other conducted in accordance with GB/T 613-2007 in.
6.6 Determination of sulphates
6.6.1 Method summary
In acidic (HCl) solution, and barium sulfate in the sample to generate a white precipitate barium sulfate, turbidity compared with the standard solution,
Do limited testing.
6.6.2 Reagents
6.6.2.1 hydrochloric acid solution. 1 + 4;
6.6.2.2 barium chloride solution. 250g/L;
6.6.2.3 sulphate (SO4) standard solution. 0.1mg/mL.
6.6.3 Analysis of step
Weigh 1g laboratory samples, accurate to 0.01g, placed in 50mL colorimetric tube, while the amount of (2 ± 0.02) mL sulphate (SO4)
Standard solution was placed in another 50mL colorimetric tube. Two colorimetric tubes were added 0.5mL of hydrochloric acid solution, 1mL barium chloride solution,
Diluted with water to the mark. After standing 10min observation, turbidity of the sample solution is not to be generated deep in turbidity standard turbidity solution produced.
6.7 Determination of chloride content
Weigh 1.0g laboratory samples, accurate to 0.01g. 0.4mL amount of chloride (Cl) standard solution (chloride containing 0.04mg) system
Preparation limits fluid. Samples showed turbidity shall not exceed the standard. Other conducted in accordance with GB/T 9729-2007 of.
6.8 Determination of Arsenic
Weigh 1.0g sample processing of laboratory samples, accurate to 0.01g, was added 5mL of water dissolved, 0.4g/L bromophenol blue indicator solution
1 drop, then a solution of (1 + 4) aqueous ammonia solution and to the solution was purple, shake. Amount of (2 ± 0.02) mL (arsenic 2.0μg) arsenic (As) standard solution
Were prepared limits. Other conducted in accordance with GB/T 5009.76-2003 Gutzeit method.
6.9 Determination of Heavy Metals
6.9.1 Method summary
Under weakly acidic (pH 3 to 4) conditions of heavy metal ions in the sample and the role of hydrogen sulfide to produce brown-black, with the same treatment of
Comparison of lead standard solution, to do limited testing.
6.9.2 Reagents
6.9.2.1 acetic acid solution. 1 + 19;
6.9.2.2 ammonia solution. 2 + 3;
6.9.2.3 sodium sulfide solution. Weigh 5g of sodium sulfide, accurate to 0.01g, with a mixture of 10mL water and 30mL glycerol dissolved into
Brown bottle. Formulated valid for three months;
6.9.2.4 phenolphthalein indicator solution. 10g/L;
6.9.2.5 Lead (Pb) standard solution. 0.01mg/mL. Before use with water 0.1mg/mL of lead (Pb) diluting the standard solution.
6.9.3 Sample Preparation
Weigh 1g laboratory samples, accurate to 0.01g, placed in 50mL colorimetric tube, add water to dissolve 25mL, add 1 drop of phenolphthalein indicator
Liquid, dropping ammonia solution to the solution was slightly red, plus 2mL acetic acid solution, shake, as the test solution.
6.9.4 Analysis of step
Take another 50mL colorimetric tube was added (1 ± 0.02) mL of lead (Pb) standard solution, then add 2mL of acetic acid and water to 25mL, shake
Uniform, as a comparative solution.
After two colorimetric tubes each added 2 drops of sodium sulfide solution, and add water to 50mL volume, and mix in a dark place 5min, in the absence of sunlight
Direct case on white background axial and lateral observation, the color of the test solution must not be darker than the color comparison solution.
6.10 Determination of Lead
6.10.1 Atomic Absorption Spectrometry
Sample processing according to GB/T 5009.75-2003 carried out in the dry digestion 5.2.2. Other press GB/T 5009.12-2003 atomic absorption
Provision income spectroscopy method.
6.10.2 colorimetry (Arbitration Act)
Press the "dry digestion" Treatment of samples. Before use, diluting lead standard solution of 1mg/mL of a standard solution of 5μg/mL of. Measurement
Timing amount of (25 ± 0.02) mL sample solution (equivalent to 2.5g laboratory sample) and (1 ± 0.02) mL of lead standard solution (equivalent to
5μgPb), were placed in 125mL separating funnel, lead standard solution was added mass fraction of 1% nitric acid to 25mL. Other Press
GB/T 5009.75-2003 of regulations.
6.11 Determination of residue on ignition
Weigh 2.5g laboratory samples, accurate to 0.001g. The arithmetic average of the results of two parallel determination of the measurement results, the two flat
Row absolute difference between the measurement result is not more than 0.02%. Other carried by GB/T 9741-1988 requirements.
6.12 Clarity test
6.12.1 Method summary
The sample was dissolved in water, and the standard solution were compared turbidimetry.
6.12.2 Reagent
6.12.2.1 nitrate solution. 1 + 2;
6.12.2.2 dextrin solution. 20g/L;
6.12.2.3 silver nitrate solution. 20g/L;
6.12.2.4 hydrochloric acid standard solution. [Ba (HCl) = 0.1mol/L];
6.12.2.5 turbidity standard solution. chlorine (Cl) 0.01mg/mL. Amount of Ba (HCl) = 0.1mol/L hydrochloric acid standard volumetric solution (14.1 ±
0.02) mL, a 50mL volumetric flask, dilute to the mark. Amount of the solution (10 ± 0.02) mL in 1000mL volumetric flask, add water
Dilute to the mark.
6.12.3 analysis step
Weigh about 1.0g laboratory samples, accurate to 0.01g, placed colorimetric tube, add 20mL of water to dissolve, as the test solution; the other to take
A colorimetric tube, was added 0.50mL accurate turbidity standard solution, add water to 20mL, add 1mL nitric acid solution, and 0.2mL dextrin solution
1mL silver nitrate solution, shake, dark place 15min, as a standard turbidity solution.
In the absence of direct sunlight, axial and lateral observation, turbidity test solution is not greater than the standard nephelometric turbidity of the solution.
6.13 Determination of fumaric acid and maleic acid content
6.13.1 Method summary
By high performance liquid chromatography, under the selected operating conditions, the sample solution through the column in each fractionation, with UV absorbance detector
Detected by external standard, the samples of fumaric acid and maleic acid content.
6.13.2 Reagent
6.13.2.1 fumaric acid. mass fraction ≥99.0%;
6.13.2.2 maleic acid. mass fraction ≥99.0%;
6.13.2.3 sodium hydroxide solution. 20g/L;
6.13.2.4 phosphoric acid solution. amount of phosphoric acid (excellent pure reagent) (1 ± 0.02) mL in 1000mL volumetric flask, add 100mL of methanol
(HPLC grade reagent) (amount can be adjusted according to the column efficiency), diluted with water to the mark, and then 0.45μm membrane filter.
6.13.3 Instruments
6.13.3.1 performance liquid chromatography system (HPLC)
6.13.3.1.1 high-pressure pump. no pulse, capable of maintaining the flow rate at 0.1mL/min ~ 10.0mL/min;
6.13.3.1.2 Loop. 5μL;
6.13.3.1.3 UV Detector. variable wavelength;
6.13.3.1.4 data processing system. a Milennium32 analysis software or the corresponding function or chromatography workstation data at
Riki.
6.13.3.2 filtration system
A pore diameter of 0.45μm filtration system using a cellulose ester membrane filter (pretreated for mobile phase).
6.13.3.3 filtration system
0.45μm pore size of the filtration system using a cellulose ester membrane filter (used for sample pretreatment).
6.13.3.4 Trace Syringe
HPLC dedicated, 50μL, 100μL (or autosampler).
6.13.4 chromatographic conditions
Recommended columns and typical operating conditions are shown in Table 2, fumaric acid and maleic acid content was measured by HPLC typically see Figure in Appendix A
Figure A. 1, the relative retention times of the components in Appendix A, Table A. 1. Others can achieve the same degree of separation columns and chromatographic run
Conditions can be used.
Table 2 column chromatography and typical operating conditions
Column
Column length 250mm, column diameter 4.6mm, silica gel as a substrate, the surface functional groups bonded to C8 nonpolar fill
Column material
Column temperature at room temperature ~ 60 ℃, control accuracy ± 1 ℃
Phosphoric acid mobile phase
Flow rate/(mL/min) 1.0
Detector wavelength/nm 214
Injection volume/μL 5
6.13.5 analysis step
Preparation of the standard sample solution 6.13.5.1
Preparation of the standard sample solution fumaric 6.13.5.1.1
Weigh 50mg fumaric, accurate to 0.0002g, is dissolved in suitable amount of water (a small amount of sodium hydroxide solution was added, if necessary), transferred to a 50mL
Volumetric flask, and dilute to scale with phosphoric acid solution.
Pipette above solution (1 ± 0.02) mL, a 50mL volumetric flask, dilute to the mark with a phosphoric acid solution, shake, filter through 0.45μm
Filtered, and ultrasonic degassing.
Preparation 6.13.5.1.2 maleic acid standard sample solution
Weigh 50mg maleic acid, accurate to 0.0002g, dissolved in an appropriate amount of water (a small amount of sodium hydroxide solution, if necessary), transferred to
250mL volumetric flask, dilute to scale with phosphoric acid solution.
Pipette above solution (1 ± 0.02) mL, placed in 100mL flask, diluted phosphoric acid solution to the mark, shake, filter through 0.45μm
Filtered, and ultrasonic degassing.
6.13.5.2 Preparation of sample solution
Weigh 0.2g laboratory samples, accurate to 0.0002g, set 50mL volumetric flask, dilute to the mark with mobile phase, shake, dried
0.45μm membrane filter, and then by ultrasonic degassing.
6.13.5.3 Determination
By HPLC procedures warm-up, adjust the temperature and flow, to analyze the conditions and steady baseline, the standard sample solution
Liquid injection.
With micro syringe (HPLC-specific) take the standard sample solution 5μL, injection (or autosampler), recording or maleic resulting fumarate
Acid peak area A2.
Using a micro syringe (HPLC-specific) sample solution 5μL, injection (or sample), and record the peak area of the test substance
Product A1.
6.13.6 Calculation Results
Calculate the mass fraction of fumaric acid or maleic acid, according to the chromatogram peak area of each component 2, the value is expressed in% according to equation (3) Calculated.
100 (3)
Where.
A1 --- sample solution peak area of the test substance;
A2 --- standard sample solution of fumaric acid or maleic acid peak area;
7 Inspection rules
7.1 product testing
Product testing and factory inspection sub-type test.
7.1.1 factory inspection
Table 1 L- malic acid (C4H6O5 meter) mass fraction, specific rotation, Sulfate (SO4 meter) mass fraction of chloride
(Cl) mass fraction, arsenic (As) content of heavy metals (Pb) content, the mass fraction of residue on ignition, Clarity test,
The mass fraction of fumaric acid and maleic acid content of the factory inspection items. Batch should be tested.
7.1.2 Type inspection
Table 1. All items are type inspection items. Under normal circumstances, at least once a month type test. The following situation
When one of the conditions, type inspection should be carried out.
a) identification of new products into production time;
b) raw materials, technology, equipment major changes that may affect product performance;
c) shut down more than three months to resume production;
d) factory inspection results are quite different and the last type inspection;
Provisions e) contract.
7.2 Batch
In each class of products or product mix shift by batch.
7.3 Sampling
According to GB/T 6678 to determine the number of sampling units, sampling according to the provisions of GB T 6679 /. The samples were mixed by quartering reduced to not
Less than 200g, packed in two clean, dry seal sample bags, stickers, ready to label stating the product name, batch number, production date on labels,
Bag for inspection by, another bag as a reserve sample stored for future reference.
7.4 Quality Certificate
Food additives L- malic acid production plant by the quality inspection department inspection in accordance with this standard, the manufacturer shall ensure that the factory's products are in line with
Requirements of this standard, each batch of products should be accompanied by a certificate of quality of a certain format, which includes. the production plant name, product name, production
Lot number or production date and serial number of this standard and so on.
7.5 determine the rules and re-examination
Test results determined in accordance with GB/T 1250 in the rounding value comparison method, the test results if there is a target does not meet the requirements of this standard
It should be twice the amount of packaging from re-sampling unit be retested, even if only an indicator of the test results do not meet the requirements of this standard, then the whole batch
Substandard products.
8 signs, packaging, transportation and storage
8.1 mark
Food additives L- malic acid containers should be securely obvious signs, including. product name, manufacturer name and address, and Suppliers
Standard, "food additive" words, food hygiene license number, production license number, lot number or production date, net content, shelf life and product quality
Demonstrate compliance with this standard and this standard number.
8.2 Packaging
Food additives L- malic acid lined with double food-grade polyethylene plastic bags cardboard drums packaging. Net weight per barrel 25kg, can also be
Packaging according to customer requirements.
8.3 Transportation and storage
Food additives should be stored in a cool, dust, dry dedicated warehouse. During transport to prevent sun, rain, Transportation to clear
Clean, to prevent bag breakage. From toxic, harmful, corrosive substances and other pollutants mixed silage during storage, transportation mix.
8.4 Shelf Life
In line with the standard packaging, transport and storage conditions, from the date of production, food additives L- malate shelf life of 24
month. Than shelf-life re-inspection, testing results meet the requirements of this standard when the product can still be used.
Book GB 13737-2008
Appendix A
(Informative)
Fumaric acid and maleic acid content was measured by high performance liquid chromatogram and typical relative retention times
A. 1 Figure A. 1 shows the determination of fumaric acid and maleic acid typical HPLC chromatograms.
1,4,5,8,9 --- unknown peaks;
2 --- L- malic acid;
3 --- maleic acid;
6 --- succinic acid;
7 --- fumaric acid.
Figure A. 1 Determination of fumaric acid and maleic acid content of a typical high-performance liquid chromatogram
A. 2 Table A. 1 shows the relative retention times of the components.
Table A. Relative retention times of the components 1
Ingredient name order peak relative retention time
1,4,5,8,9 unknown peaks -
2 L- malic acid 1
3 maleate 1.40
Succinic 6 1.70
7 fumaric 1.80
8002-
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