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GB 1903.45-2020: National food safety standard - Food nutritional fortification substance - Nicotinamide
GB 1903.45-2020
GB
NATIONAL STANDARD OF THE
PEOPLE?€?S REPUBLIC OF CHINA
National Food Safety Standard - Food Nutritional
Fortification Substance - Nicotinamide
ISSUED ON: SEPTEMBER 11, 2020
IMPLEMENTED ON: MARCH 11, 2021
Issued by: National Health Commission of the PRC;
State Administration for Market Regulation.
Table of Contents
1 Scope ... 3
2 Chemical Name, Structural Formula, Molecular Formula and Relative
Molecular Mass ... 3
3 Technical Requirements ... 3
Appendix A Inspection Methods ... 5
Appendix B Infrared Spectrum of Nicotinamide Standard Substance, and Liquid
Chromatogram of Nicotinamide Solution ... 16
National Food Safety Standard - Food Nutritional
Fortification Substance - Nicotinamide
1 Scope
This Standard is applicable to the food nutritional fortification substance of
nicotinamide obtained and produced through corresponding chemical synthetic
process, and take methyl nicotinate (or ethyl nicotinate, or 3-methylpyridine, or 3-
cyanopyridine, or 5-pentanediamine, 2-methyl-1) as the raw material.
2 Chemical Name, Structural Formula, Molecular
Formula and Relative Molecular Mass
2.1 Chemical name
3-pyridine-carboxamide
2.2 Structural formula
2.3 Molecular formula
C6H6N2O
2.4 Relative molecular mass
122.13 (according to 2018 international relative atomic mass)
3 Technical Requirements
3.1 Sensory requirements
The sensory requirements shall comply with the provisions of Table 1.
Appendix A
Inspection Methods
A.1 General rules
When other requirements are not specified, the reagents and water that are used in
this Standard refer to analytically pure reagents and the Class-III water specified in
GB/T 6682. When other requirements are not specified, the standard solutions,
preparations, and products that are used in the test shall be prepared according to the
provisions of GB/T 601, GB/T 602, GB/T 603. When the solutions that are used in the
test are not specified by which solvent to prepare, they all indicate the aqueous solution.
A.2 Identification test
A.2.1 Color reaction
A.2.1.1 Reagents and materials
A.2.1.1.1 Sodium hydroxide solution: Take 4.3g of sodium hydroxide; add 100mL of
water; stir to dissolve and mix evenly.
A.2.1.1.2 Phenolphthalein indicator solution.
A.2.1.1.3 Sulfuric acid solution: Take 57mL of sulfuric acid; slowly add it to water; and
dilute to 1000mL by water and mix evenly.
A.2.1.1.4 Copper sulfate solution: Take 12.5g of copper sulfate pentahydrate; add
100mL of water; and stir to dissolve and mix evenly.
A.2.1.2 Analysis procedures
Take 0.1g of specimen (accurate to 0.01 g); add 5mL of water to dissolve; add 5mL of
sodium hydroxide solution; and slowly heat it to generate ammonia gas and make the
wet red litmus paper turn blue (the difference from niacin). Continue heating until the
ammonia odor is completely removed; let it cool; add 1 ~ 2 drops of phenolphthalein
indicator solution; neutralize by sulfuric acid solution; and add 2mL of copper sulfate
solution; a light blue precipitate shall slowly precipitate.
A.2.2 Infrared spectrum test
Use the potassium bromide pellet technique to test in accordance with GB/T 6040. The
infrared spectrogram of the specimen shall be consistent with that of the nicotinamide
standard substance (see Figure B.1)
detector.
A.3.2.2 Potentiometric titrator.
A.3.2.3 Electronic balance: the accuracy is 0.0001 g
A.3.2.4 pH meter: the accuracy is 0.01.
A.3.3 Analysis procedures
A.3.3.1 Perchloric acid titration method
A.3.3.1.1 Indicator titration method
A.3.3.1.1.1 Method summary
Use crystal violet as an indicator; titrate the specimen with perchloric acid standard
solution; and calculate the nicotinamide content based on the amount of the consumed
perchloric acid standard titrant.
A.3.3.1.1.2 Analysis procedures
Take 0.1g of specimen (accurate to 0.0001g); add 30mL of glacial acetic acid to
dissolve it (if necessary, warm it up to dissolve it completely). Add 1 drop ~ 2 drops of
crystal violet indicator solution; titrate with perchloric acid standard titration solution
until the solution turns blue-green and does not fade within 30s, which is the end point
of the titration. Do a blank test at the same time.
A.3.3.1.2 Potentiometric titration method
A.3.3.1.2.1 Method summary
Take calomel electrode as reference electrode, non-aqueous acid-base titration glass
electrode as indicator electrode; and titrate the specimen with perchloric acid standard
solution. According to the potential "jump", determine the titration end point. According
to the amount of consumed perchloric acid standard titrant, calculate the nicotinamide
content.
A.3.3.1.2.2 Analysis procedures
Take 0.1g of specimen (accurate to 0.0001 g); add 30mL of glacial acetic acid to
dissolve it (if necessary, slightly warm it to dissolve it completely; if glacial acetic acid
cannot flood the electrode, add glacial acetic acid appropriately). Use a potentiometric
titrator to titrate by a perchloric acid standard titration; and do a blank test at the same
time.
A.3.3.2 Liquid chromatography
As - the peak area of nicotinamide in the standard substance solution;
m ?€? the mass of the specimen, in g;
w ?€? mass fraction of the specimen drying loss, in %;
100 ?€? coefficient, the results shall be converted into %;
1000 ?€? conversion coefficient, convert mg into g.
The test results are based on the arithmetic mean of the parallel determination results.
The absolute difference between two independent determination results obtained
under repeatability conditions shall be no more than 0.5% of the arithmetic mean.
A.4 Determination of absorption coefficient E1% 1cm (261nm)
A.4.1 Method principle
The purity of the specimen shall be expressed by measuring the absorption coefficient
of the specimen solution at a specific wavelength.
A.4.2 Reagents and materials
Hydrochloric acid solution: 0.1 mol/L.
A.4.3 Apparatus
A.4.3.1 1 cm quartz cuvette.
A.4.3.2 UV spectrophotometer.
A.4.3.3 Electronic balance with an accuracy of 0.0001 g.
A.4.4 Analysis procedures
Accurately take 0.15g of specimen (accurate to 0.0001g); use the hydrochloric acid
solution to make constant volume of 100 mL; and mix evenly. Then take another
1.00mL into a 100mL volumetric flask; add hydrochloric acid solution to make the
constant volume to the mark; and mix evenly. That is the specimen solution. Pour the
specimen solution into a 1cm quartz cuvette; use the hydrochloric acid solution as the
reference solution; use a spectrophotometer to measure absorption coefficient (E1% 1cm)
at a wavelength of 261nm.
A.4.5 Calculation of results
The absorption coefficient E1% 1cm is calculated according to Formula (A.3):
A.8.1 Method summary
Dissolve the specimen in a sulfuric acid solution; and compare it with the control
solution; its color shall not be darker.
A.8.2 Reagents and materials
A.8.2.1 Sulfuric acid.
A.8.2.2 Ammonia test solution: Take 40 mL of concentrated ammonia water; dilute to
100 mL with water; and mix evenly.
A.8.2.3 Hydrochloric acid: analytically pure.
A.8.2.4 Colorimetric cobalt chloride solution: Weigh 32.5g of cobalt chloride
hexahydrate (CoCl2 ?€? 6H2O) (accurate to 0.0001g); add an appropriate amount of
hydrochloric acid solution (1 ??? 40) to dissolve it into 500mL. Then take 2.00mL; place
it in a conical flask; add 200mL of water to mix evenly; add ammonia solution until the
solution turns from light red to green. Add 10mL of acetic acid-sodium acetate buffer
solution (pH 6.0); and heat to 60 ??C. Add 5 drops of xylenol orange indicator solution;
and titrate with edetate disodium titration solution (0.05 mol/L) until it appears yellow.
Each 1 mL of edetate disodium titration solution (0.05 mol/L) is equivalent to 11.90mg
of cobalt chloride hexahydrate. According to the above measurement results, add an
appropriate amount of hydrochloric acid solution (1 ??? 40) to the remaining original
solution; so that each 1 mL of the solution contains 59.5mg of cobalt chloride
hexahydrate; then the solution is obtained.
A.8.2.5 Colorimetric potassium dichromate solution: Take 0.4g of reference potassium
dichromate (accurate to 0.0001g) dried at 120 ??C to constant weight; place it in a
500mL volumetric flask; and add appropriate amount of water to dissolve and dilute to
the mark; shake well; then the solution is obtained. Each 1 mL of the solution contains
0.800mg of potassium dichromate (K2Cr2O7).
A.8.2.6 Colorimetric copper sulfate solution: Take 32.5g of copper sulfate pentahydrate
(accurate to 0.001 g); add an appropriate amount of hydrochloric acid solution (1 ???
40) to dissolve it into 500mL. Then take 10.00 mL; and place it into the iodine flask;
add 50mL of water, 4 mL of acetic acid (glacial acetic acid) and 2g of potassium iodide.
Then titrate with sodium thiosulfate titrant (0.1 mol/L). When it is near the end point,
add 2mL of starch indicator solution and continue titrate until the blue color disappears.
Each 1 mL of sodium thiosulfate titrant (0.1 mol/L) is equivalent to 24.97mg of CuSO4
?€? 5H2O. According to the above measurement results, add an appropriate amount of
hydrochloric acid solution (1 ??? 40) to the remaining original solution; so that each 1
mL of the solution contains 62.4 mg of CuSO4 ?€? 5H2O; and the solution is obtained.
A.8.2.7 Control solution: Take 1.0 mL of colorimetric cobalt chloride solution, 2.5 mL of
colorimetric potassium dichromate solution, and 1.0 mL of colorimetric copper sulfate
40mg); and take it as specimen solution A. Take 0.5mL of specimen solution A; add
anhydrous ethanol and make constant volume to 100 mL, which is the control solution
(I). Take 10 mL of control solution (I); dilute with ethanol and make constant volume to
20 mL, which is control solution (II).
A.9.3.1.2 Take 0.1g of niacin (accurate to 0.001g); add anhydrous ethanol to dissolve
and make constant volume to 50mL; mix evenly; then obtain the niacin intermediate
stock solution. Pipette 2.5mL of the niacin intermediate stock solution; dilute with
anhydrous ethanol and make constant volume to 25 mL; mix evenly (each 1mL of the
solution contains approximately 0.2mg of niacin); then obtain the reference solution.
A.9.3.1.3 Respectively, take 10mL of niacin intermediate stock solution (A.9.3.1.2),
2.5mL of specimen solution A; mix evenly; dilute with anhydrous ethanol and make
constant volume to 100 mL; then obtain the control solution (III).
A.9.3.2 Analysis procedures
Respectively pipette 5??L of specimen solution A, control solution (I), control solution
(II), control solution (III), and reference solution in A.9.3.1; and respectively place them
on the same silica gel GF254 thin-layer board above; take chloroform-anhydrous
ethanol-water (48:45:4) as developing agent; unfold; dry; and inspect under ultraviolet
lamp (254 nm).
A.9.3.3 Judgment of results
The control solution (III) shall display two clearly separated spots; the control solution
(II) shall display a clearly visible spot. If the specimen solution A displays impurity spots
corresponding to the reference solution, its color shall be no darker than that of the
main spots of the reference solution. If the specimen solution A displays other impurity
spots, compared with the main spots of the control solution (I), when the color of
impurity spots displayed by the specimen solution A is no darker than that of the main
spots of control solution (I), it shall pass the test.