GB 30602-2014_English: PDF (GB30602-2014)
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National Food Safety Standard -- Food Additives -- Sodium Ethyl p-hydroxybenzoate
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GB 30602-2014
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Standard ID | GB 30602-2014 (GB30602-2014) | Description (Translated English) | National Food Safety Standard - Food Additives - Sodium Ethyl p-hydroxybenzoate | Sector / Industry | National Standard | Classification of Chinese Standard | X09 | Classification of International Standard | 67.02 | Word Count Estimation | 9,911 | Date of Issue | 2014/4/29 | Date of Implementation | 2014/11/1 | Administrative Organization | National Health and Family Planning | Regulation (derived from) | National Health and Family Planning Commission Bulletin No. 7, 2014 | Issuing agency(ies) | National Health and Family Planning Commission of the People's Republic of China | Summary | This Standard specifies the sodium hydroxide solution were added to a food additive reaction after Ethylparaben refined Ethylparaben sodium. |
GB 30602-2014
(Food Additives Sodium Ethylparaben)
National Standards of People's Republic of China
National standards for food safety
Food Additives Ethyl p-hydroxybenzoate
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 Ethyl p-hydroxybenzoate
1 Scope
This standard applies to sodium hydroxide in aqueous solution by adding ethyl p-hydroxybenzoate after the reaction of refined food additives p-hydroxybenzene
Ethyl formate sodium.
2 chemical name, molecular formula, structural formula and relative molecular mass
2.1 Chemical name
Ethyl p-hydroxybenzoate.
2.2 Molecular formula
C9H9NaO3.
2.3 Structural formula
2.4 Relative molecular mass.
188.2 (according to.2007 International relative atomic mass)
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, in the natural 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
Ethyl p-hydroxybenzoate Sodium content (dry basis) (mass fraction) /% 99.0 to 103.0 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 ≤ through 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 ethyl 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 115 ℃ ~ 118 ℃.
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 ethyl 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 sodium 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 --- the value of the mass of the sample after conversion to dry basis, in grams (g);
M - the molar mass of sodium p-hydroxybenzoate in parts per gram (g/mol) [M (C9H9NaO3) =
188.2];
1000 --- conversion factor.
The results of the test are based on the arithmetic mean of the parallel measurement results (leave a decimal). Two independent tests obtained under repetitive conditions
The absolute difference between the results 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 Ethyl p-hydroxybenzoate Standard. Mass fraction ≥95%.
A.6.2.2 p-hydroxybenzoic acid standards. 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 micro-injector, 50 μL.
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
The column octadecyl silane bonded silica was a stationary phase
Mobile phase methanol. acetic acid solution = 60.40
Detector detection wavelength/nm 254
Injection volume/μL 20
Column temperature/℃ room temperature, not more than 40 ℃
A.6.5 Analysis steps
A.6.5.1 Preparation of mixed solution of ethyl p-hydroxybenzoate and p-hydroxybenzoic acid
Respectively, appropriate amount of ethyl p-hydroxybenzoate and p-hydroxybenzoic acid, mixed with mobile phase dissolved and diluted to produce containing p-hydroxybenzene
Ethyl formate, and 0.1 mg/mL of p-hydroxybenzoic acid.
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
Press the high performance liquid chromatography procedure to adjust the instrument to make the baseline smooth. Take 20 μL of ethyl p-hydroxybenzoate and p-hydroxybenzoic acid
Mixed solution into the chromatograph, record the chromatogram, the theoretical number of sodium p-hydroxybenzoate sodium concentration of not less than 8000, p-hydroxybenzoic acid
Ethyl ester sodium peak and the separation of p-hydroxybenzoic acid peak should be greater than 1.5. Add 20 μL of the control solution to adjust the detection sensitivity to make the hydroxybenzene
The sodium peak of ethyl acetate is about 20% of full scale. 20 μL of the control solution and the sample solution were accurately injected, and the chromatogram was recorded to the hydroxyl group
4 times the retention time of sodium benzoate sodium.
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 sodium p-hydroxybenzoate sodium peak
Plot 4 times. Other single impurity peak area shall not be greater than 0.5 times the peak area of ethyl p-hydroxybenzoate in the control solution. Other miscellaneous
The area of the peak area is not greater than the peak area of sodium 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 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) was prepared in a solution containing 59.5 mg/mL of cobalt chloride hexahydrate (CoCl2 · 6H2O).
A.7.1.3 Preparation of standard colorimetric solutions
Accurate measurement of 12.0mL colorimetric with cobalt chloride solution, 20.0mL color with potassium dichromate solution and 68.0mL water, mix shake, as
Standard stock solution. Accurately measure 2.5mL standard stock solution, add 7.5mL water, mix and shake, the standard colorimetric solution.
A.7.2 Analysis steps
Weighed 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 on the same white background, from top to bottom perspective, or with the same white background, head view, try
The color of the sample tube is not deeper than the control tube.
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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