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GB 30601-2014: National Food Safety Standard -- Food Additives -- Sodium Ethyl p-hydroxybenzoate
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National Food Safety Standard -- Food Additives -- Sodium Ethyl p-hydroxybenzoate
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GB 30601-2014
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Basic data | Standard ID | GB 30601-2014 (GB30601-2014) | | Description (Translated English) | National Food Safety Standard -- Food Additives -- Sodium Ethyl p-hydroxybenzoate | | Sector / Industry | National Standard | | Classification of Chinese Standard | C53 | | Classification of International Standard | 67.020 | | Word Count Estimation | 9,919 | | Date of Issue | 4/29/2014 | | Date of Implementation | 11/1/2014 | | Regulation (derived from) | National Health and Family Planning Commission Bulletin No. 7, 2014 | | 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 Standard specifies the addition of food additives benzoate reaction after refining of sodium methyl benzene by sodium hydroxide solution. | GB 30601-2014: National Food Safety Standard -- Food Additives -- Sodium Ethyl p-hydroxybenzoate
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(Food additive sodium methylparaben)
National Standards of People's Republic of China
National standards for food safety
Food additives methyl p-hydroxybenzoate sodium
Released.2014-04-29
2014-11-01 implementation
People's Republic of China
National Health and Family Planning Commission released
National standards for food safety
Food additives methyl p-hydroxybenzoate sodium
1 Scope
This standard applies to sodium hydroxide in aqueous solution by adding methyl p-hydroxybenzoate after the reaction of refined food additives p-hydroxybenzene
Methyl formate sodium.
2 chemical name, molecular formula, structural formula and relative molecular mass
2.1 Chemical name
Methyl p-hydroxybenzoate.
2.2 Molecular formula
C8H7NaO3.
2.3 Structural formula
2.4 Relative molecular mass
174.15 (according to.2007 International Relative Atomic Quality).
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 or near white
State powder
Take appropriate sample, placed in a clean, dry white porcelain dish, observed under natural light
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
Methyl p-hydroxybenzoate (on a dry basis) (mass fraction) /% 98.5 to 101.5 Appendix A, A.3
Moisture (mass fraction) /% ≤ 5.0 GB 5009.3 Karl Fischer method
pH (1 g/L aqueous solution) 9.5 to 10.5 GB/T 9724 (0.10 g sample, dissolved in 100 mL water)
Chloride (in Cl-terms) (mass fraction) /% ≤ 0.035 A.4
Sulfate (in terms of SO2-4) (mass fraction) /% ≤ 0.030 A.5
Impurities
P-hydroxybenzoic acid (mass fraction) /% ≤ 4.0
Other single impurities (mass fraction) /% ≤ 0.5
The sum of other single impurities (mass fraction) /% ≤ 1.0
A.6
The clarity and color of the solution passed the test A.7
Lead (Pb)/(mg/kg) ≤ 2 A.8
Appendix A
Testing method
A.1 General provisions
Unless otherwise stated, only the reagents identified as analytical reagents and the tertiary water specified in GB/T 6682 were used in the analysis.
Standard titration solution, impurity standard solution, preparation and products used in the analysis, in the absence of other requirements, according to GB/T 601,
GB/T 602 and 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.2 Identification test
A.2.1 Reagents and materials
A.2.1.1 Hydrochloric acid.
A.2.1.2 Hydrochloric acid solution. 1 1.
A.2.1.3 Sodium carbonate solution. 106 g/L.
A.2.1.4 Potassium ferricyanide solution. 53 g/L.
A.2.1.5 4-Amino Antipyrine-Borate Buffer Solution. 0.1%.
1000 mL of 0.1 mol/L potassium chloride solution containing 0.618% boric acid was mixed with 420 mL of 0.1 mol/L sodium hydroxide solution,
A borate buffer solution of pH 9.0 was obtained.
Take 1 g of 4-aminoantipine in 1000 mL of borate buffer solution.
A.2.1.6 uranyl zinc acetate solution.
Weigh 10g uranyl acetate, add 5mL glacial acetic acid and 50mL water, slightly heat to dissolve; weighed 30g zinc acetate, add 3mL ice B
Acid and 30mL water, slightly heat to dissolve; the two solutions mixed, let cool, filter, that is, too.
A.2.2 Identification steps
A.2.2.1 Melting point of methyl p-hydroxybenzoate
Weigh 0.5g sample, accurate to 0.01g, add 50mL of water to dissolve, add 5mL hydrochloric acid immediately, shake, filter, wash with water
The precipitate was dried at 80 ° C for 2 hours under reduced pressure. According to GB/T 617 determination of the melting point of the sample, the melting point of 125 ℃ ~ 128 ℃.
A.2.2.2 Color reaction
Take 0.01g sample, placed in a test tube, add 1mL sodium carbonate solution, heating and boiling for 30s, cooling, adding 5mL4-amino antipyil
Forest - borate buffer solution and 1mL potassium ferricyanide solution, mix, the solution becomes red.
A.2.2.3 Sodium salt test
Platinum wire moist with hydrochloric acid, dipped in samples, burning in a colorless flame, the flame should be bright yellow.
Weigh 1g sample, accurate to 0.01g, with the appropriate amount of water dissolved, add 1mL hydrochloric acid solution, diluted with water to 20mL. Take 1mL of the
Sample solution, add 5mL uranyl acetate zinc solution, shake, a yellow precipitate produced.
A.3 Determination of sodium content of methyl p-hydroxybenzoate
A.3.1 Reagents and materials
A.3.1.1 Glacial acetic acid.
A.3.1.2 Standard titration solution for perchloric acid. c (HClO4) = 0.1 mol/L.
A.3.2 Analysis steps
Weigh about 0.15g sample, accurate to 0.0001g, add 50mL glacial acetic acid dissolved, titration with titanate titration solution, the potential drop
The law indicates the end point. While the blank test.
A.3.3 Calculation of results
The mass fraction w1 of methyl p-hydroxybenzoate (dry basis) is calculated according to formula (A.1)
w1 =
(V1-V2) × c × M
m × 1000 ×
100% (A.1)
Where.
V1 --- blank consumption Perchloric acid standard titration solution volume value in milliliters (mL);
V2 --- sample consumption Perchloric acid standard titration solution volume value in milliliters (mL);
c - the exact value of the perchloric acid standard titration solution concentration in moles per liter (mol/L);
M-methyl p-hydroxybenzoate sodium (C8H7NaO3), in grams per mole (g/mol)
(M = 174.1);
m --- the value of the mass of the sample after conversion to dry basis, in grams (g);
1000 --- conversion factor.
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 1.0%.
A.4 Determination of Chloride
A.4.1 Reagents and materials
A.4.1.1 Nitric acid solution. 1 9.
A.4.1.2 Silver nitrate solution. 17 g/L.
A.4.1.3 Chloride (Cl-) standard solution. 0.01 mg/mL.
A.4.2 Analysis steps
Weigh 2.0g sample, add 40mL water dissolved, with nitric acid solution to adjust the solution to neutral, diluted with water to 50mL, shaking, filtering,
Retention filtrate. Take the filtrate 5.0mL, as the test solution, placed in 50mL Na colorimetric tube, add 10mL nitric acid solution, add water to the volume of about
40mL, add 1.0mL silver nitrate solution, diluted with water to 50mL, shake, dark place for 5min, in the black background, axial observation, try
The turbidity of the solution shall not exceed the standard.
The standard is to measure 7.0mL chloride (Cl-) standard solution, the same with the test solution at the same time.
A.5 Determination of Sulfate
A.5.1 Reagents and materials
A.5.1.1 hydrochloric acid solution. 1 3.
A.5.1.2 Barium chloride solution. 250 g/L.
A.5.1.3 Potassium Sulfate Standard Solution. 0.1 mg/mL.
A.5.2 Analysis steps
Measure the filtrate of A.4.2 25mL, as the test solution, placed in 50mL Na colorimetric tube, add 2mL hydrochloric acid solution, add water to the body
Plot about 40mL, add 5mL barium chloride solution, diluted with water to 50mL, shake, place 10min, in the black background, axial observation, try
The turbidity of the solution shall not exceed the standard.
The standard is to measure 2.4mL potassium sulfate standard solution, and test solution at the same time the same treatment.
A.6 Determination of impurities
A.6.1 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
Detection of the external standard method, the sample of the impurities in the content.
A.6.2 Reagents and materials
A.6.2.1 Sodium p-hydroxybenzoate. chromatographic purity, mass fraction ≥95%.
A.6.2.2 p-hydroxybenzoic acid. mass fraction ≥99%.
A.6.2.3 Methanol.
A.6.2.4 Glacial acetic acid solution. 1 → 100.
A.6.3 Instruments and equipment
A.6.3.1 High Performance Liquid Chromatography (HPLC). equipped with a UV detector.
A.6.3.2 Sampler. Autosampler or 50 μL Micro Sampler.
A.6.3.3 Data processing systems. Chromatographic workstations or data processors.
A.6.4 Chromatographic analysis conditions
The recommended columns and typical operating conditions are shown in Table A.1. Other columns and chromatographic operating conditions that can achieve the same degree of separation
use.
Table A.1 Columns and Typical Chromatographic Operating Conditions
Project operating conditions
Column
250mm × 4.6mm (column length × column diameter) stainless steel column, octadecyl silane bonded silica as a stationary phase, particle size 3μm ~
10 μm
Mobile phase methanol. acetic acid solution = 60.40
Flow rate/(mL/min) 0.8
Column temperature/℃ room temperature, not more than 40 ℃
Detector detection wavelength/nm 254
Injection volume/μL 20
A.6.5 Analysis steps
A.6.5.1 Preparation of mixed solution of methyl p-hydroxybenzoate sodium and p-hydroxybenzoic acid
Respectively, the appropriate amount of methyl p-hydroxybenzoate sodium, p-hydroxybenzoic acid, dissolved with mobile phase, shake and dilute, made of each containing p-hydroxybenzene
Methyl formate sodium, and p-hydroxybenzoic acid 0.1 mg/mL.
A.6.5.2 Preparation of sample solutions
An appropriate sample was weighed and dissolved and diluted with a mobile phase to prepare a 1.0 mg/mL sample solution.
A.6.5.3 Preparation of Control Solution
Accurately measure the amount of sample solution, diluted with mobile phase, made of 10μg/mL of the control solution.
A.6.5.4 Determination
Control the instrument according to the high performance liquid chromatography procedure to make the baseline stable, inject 20 μL of methyl p-hydroxybenzoate sodium and p-hydroxybenzoic acid
Mixed solution, record the number of theoretical plates based on sodium p-hydroxybenzoate sodium peak of not less than 8000, methyl p-hydroxybenzoate sodium peak and
The separation of p-hydroxybenzoic acid peaks is greater than 1.5. Samples of 20 μL of the control solution were adjusted to detect the sensitivity of the methylhydroxybenzoate to the sodium peak
High about 20% of full scale. 20 μL of the control solution and the sample solution were accurately injected, and the chromatogram was recorded to sodium methyl p-hydroxybenzoate
Peak retention time 4 times.
A.6.6 Calculation of results
In the sample solution chromatogram, if the p-hydroxybenzoic acid peak, the peak area shall not be greater than the control solution of methyl p-hydroxybenzoate sodium peak
Plot 4 times. Other single impurity peak area shall not be greater than 0.5 times the peak area of methyl p-hydroxybenzoate sodium in the control solution. Other miscellaneous
The area of the peak area should not be greater than the peak area of methyl p-hydroxybenzoate in the control solution.
A.7 The clarity and color of the solution
A.7.1 Reagents and materials
A.7.1.1 Preparation of colorimetric potassium dichromate solution
Weigh 0.4000g of potassium dichromate, which was dried to constant volume at 120 ° C, placed in a 500 mL volumetric flask, dissolved in water and diluted
To the scale, shake. The solution contains potassium dichromate (K2Cr2O7) 0.800 mg/mL.
A.7.1.2 Preparation of copper sulfate solution for colorimetric use
Weigh about 32.5g copper sulfate pentahydrate, accurate to 0.01g, add appropriate amount of hydrochloric acid solution (1 → 40) dissolved, into the 500mL volumetric flask
, Diluted with hydrochloric acid solution (1 → 40) to the scale. Accurately measure 10.0mL of the solution in the iodine bottle, add 50mL of water and 4mL acetic acid,
2g potassium iodide, titration with sodium thiosulfate solution [c (Na2S2O3) = 0.1mol/L] titration, near the end point, add 2mL starch instructions
Liquid, continue to titration to blue disappear, record the consumption of sodium thiosulfate standard titration solution volume. Per 1mL sodium thiosulfate standard titration
The solution is equivalent to 24.97 mg of copper sulfate pentahydrate (CuSO4.5H2O). Based on the above titration results, in the remaining copper sulfate solution
Adding the appropriate amount of hydrochloric acid solution (1 → 40), prepared with copper sulfate pentahydrate (CuSO4 · 5H2O) 62.4mg/mL solution.
A.7.1.3 Preparation of cobalt chloride solution for colorimetric use
Weigh about 32.5g cobalt chloride hexahydrate, accurate to 0.01g, add appropriate amount of hydrochloric acid solution (1 → 40) dissolved, into the 500mL volumetric flask
, Diluted with hydrochloric acid solution (1 → 40) to the scale. Accurately measure 2.0mL of the solution in a conical flask, add.200mL water shake, add ammonia
Solution to the cobalt chloride solution from light red to green, add 10mL acetic acid - sodium acetate buffer solution (pH6.0), heated to 60 ℃, add 5 drops
Xylenol orange indicator solution, with ethylenediamine tetraacetic acid disodium standard titration solution [c (EDTA) = 0.05mol/L] titration to the solution was yellow, remember
Record the volume of sodium thiosulfate standard titration solution. The titration solution is equivalent to 11.90 mg per 1 mL of ethylenediamine tetraacetic acid disodium
Of cobalt chloride hexahydrate (CoCl2 · 6H2O). According to the above titration results, in the remaining cobalt chloride solution by adding the appropriate amount of hydrochloric acid solution
(1 → 40), prepared with a cobalt chloride hexahydrate (CoCl2 · 6H2O) 59.5mg/mL solution.
A.7.1.4 Preparation of standard colorimetric solutions
Accurate measurement of 22.5mL colorimetric with cobalt chloride solution, 12.5mL color with potassium dichromate solution, 20.0mL color with copper sulfate solution and
45.0mL water, mix and shake, as the standard color solution of the stock solution. Accurate measurement of 1.5mL standard color liquid stock solution, add 8.5mL of water,
Mix shake, the standard colorimetric solution.
A.7.2 Analysis steps
Weigh 1.0g sample, placed in 25mL Na colorimetric tube, add 10mL of water dissolved, the solution should be clear. Another standard colorimetric solution
10mL, placed in another 25mL Nessler color tube, two tubes with the same white background, from top to bottom perspective, or with the same white background,
The color of the sample solution shall not be deeper than the standard colorimetric color.
A.8 Determination of lead
According to GB 5009.12-2010 in the "graphite furnace atomic absorption spectrometry" or "flame atomic absorption spectrometry". Among them, the sample does not need
Pretreatment, sample digestion can be used according to laboratory conditions, "dry ashing" or "wet digestion method", and as the sample will sample solution into
Line proper dilution.
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