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National Food Safety Standard -- Food Additives -- L-α-aspartyl-N-(2,2,4,4-tetramethyl-3-trimethylene sulfide) -D-alaninamide (also known as alitame)
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GB 1886.99-2015
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PDF similar to GB 1886.99-2015
Basic data | Standard ID | GB 1886.99-2015 (GB1886.99-2015) | | Description (Translated English) | National Food Safety Standard -- Food Additives -- L-��-aspartyl-N-(2,2,4,4-tetramethyl-3-trimethylene sulfide) -D-alaninamide (also known as alitame) | | Sector / Industry | National Standard | | Classification of Chinese Standard | X40 | | Word Count Estimation | 9,978 | | Date of Issue | 2015-09-22 | | Date of Implementation | 2016-03-22 | | Regulation (derived from) | PRC National Health and Family Planning Commission 2015 No.8 | | Issuing agency(ies) | National Health and Family Planning Commission of the People's Republic of China |
GB 1886.99-2015: National Food Safety Standard -- Food Additives -- L-α-aspartyl-N-(2,2,4,4-tetramethyl-3-trimethylene sulfide) -D-alaninamide (also known as alitame) ---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.
(National Food Safety Standard Food Additive L-α- aspartyl -N- (2, 2, 4, 4- tetramethyl-3-trimethylene sulfide) -D- alaninamide (aka alitame))
National Standards of People's Republic of China
National Food Safety Standard
Food Additive L-α- aspartyl -N-
(2,2,4,4-tetramethyl-3-trimethylene sulfide)
-D- Alanine amide (also known as alitame)
Issued on. 2015-09-22
2016-03-22 implementation
People's Republic of China
National Health and Family Planning Commission released
National Food Safety Standard
Food Additive L-α- aspartyl -N-
(2,2,4,4-tetramethyl-3-trimethylene sulfide)
-D- Alanine amide (also known as alitame)
1 Scope
This standard applies to food additives L-α- aspartyl -N- (2,2,4,4- tetramethyl-3 trimethylene sulfide) -D- alanine amide (aka
Alitame).
2 chemical name, molecular formula, molecular mass and structural formula
2.1 Chemical Name
L-α- aspartyl -N- (2,2,4,4- tetramethyl-3 trimethylene sulfide) -D- alaninamide
Formula 2.2
C14H25N3O4S · 2.5H2O
2.3 formula
2.4 relative molecular mass
376.47 (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
Project requires test methods
Color White
Status crystalline powder
Odorless or slight odor distinctive odor.
The sample was placed in a clean, dry white porcelain dish, under natural light, observation
The state of its color, smell its odor
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
Alitame content (dry basis), w /% 98.0 ~ 101.0 Appendix A A.3
β- isomer (dry basis), w /% ≤ 0.3 Appendix A A.3
Alanine amide (dry basis), w /% ≤ 0.2 Appendix A A.3
Water, w /% 11 ~ 13 GB/T 6283
Specific rotation αm (25 ℃, D)/[(°) · dm2 · kg-1] 40 ~ 50 in Appendix A A.4
Residue on ignition, w /% ≤ 1.0 GB/T 9741a
Lead (Pb)/(mg/kg) ≤ 1.0 GB 5009.12
a burning temperature of 800 ℃ ± 25 ℃.
Appendix A
Testing method
A.1 General Provisions
This standard reagents and water in the absence of other specified requirements, refer to the three water analytical reagent and GB/T 6682 regulations. test
In the standard solution, standard solution for measuring impurities, formulations and products, did not indicate when the other requirements according to GB/T 601, GB/T 602 with
And the provisions of GB/T 603 was prepared. Solution was used in the tests did not indicate what is formulated with solvent, it refers to an aqueous solution.
A.2 Identification Test
A.2.1 solubility
Soluble in water and ethanol.
A.2.2 IR spectra
IR spectra consistent with Figure B.1.
A.2.3 pH
pH 50g/L of sample solution is 5.0 to 6.0.
A.2.4 color reaction
A.2.4.1 Weigh 300mg ninhydrin added 100mL of n-butanol and 2mL glacial acetic acid formulated as a solution, of this solution 5mL, added
10mg sample was slowly heated to reflux, should appear bright blue-purple.
A.2.4.2 Take 5mL freshly prepared c (
5KMnO4
) = Potassium permanganate standard solution 0.001mol/L, add 10mg sample and filled
Well mixed, the solution from purple to brown.
Determination A.3 alitame (dry basis) content, β- isomers and alanine amide
A.3.1 Method summary
Ion-pair reversed-phase HPLC method under the selected operating conditions, the sample solution through the column in each fractionation,
UV absorption detector, using external standard, calculate the content of the samples alitame, β- isomers and alanine amide.
A.3.2 Reagents and materials
A.3.2.1 methanol.
A.3.2.2 Acetonitrile. HPLC grade, at 210nm the light transmittance is greater than 90%.
A.3.2.3 β- isomer. standard sample.
A.3.2.4 alanine amide. standard sample.
A.3.2.5 alitame. standard sample.
A.3.2.6 buffer solution. Weigh 0.69g sodium phosphate monobasic (monohydrate) and 4.32g1- octyl sulfate, accurate to 0.0001g, placed
1000mL volumetric flask. 200mL of water was added to dissolve adjusted to pH 2.5 with phosphoric acid, diluted with water to the mark. By pore size
0.22μm millipore membrane filter or equivalent.
A.3.3 Instruments and Equipment
A.3.3.1 high performance liquid chromatography system (HPLC).
A.3.3.2 constant flow pump.
A.3.3.3 UV absorbance detector.
A.3.4 Chromatography conditions
Recommended columns and typical operating conditions are shown in Table A.1.
Table A.1 column chromatography and typical operating conditions
C18 column 15cm × 0.4cm
Column temperature room temperature
Appendix A mobile phase in A.3.5.1
Flow rate/(mL/min) 1.0
Detector wavelength/nm 217
A.3.5 Analysis step
A.3.5.1 Preparation of the mobile phase
Accurately taken acetonitrile and buffer solution volume ratio 1.3 mixed well. By vacuum degassing.
A.3.5.2 Preparation of standard working solution
A.3.5.2.1 standard solution A1. Weigh β- alanine amide isomers and each about 25mg, accurate to 0.0001g, moved 500mL capacity
Bottle. 50mL methanol was added to dissolve, dilute to the mark with water. Stored in a refrigerator.
A.3.5.2.2 standard solution A2. Pipette 15mL ± 0.02mL standard solution A1 to 50mL volumetric flask, diluted with water to the mark.
A.3.5.2.3 standard solution W1. Weigh about 50mg alitame standard samples, accurate to 0.0001g, moved into 10mL volumetric flask,
Add 5mL standard solution A2, diluted with water to the mark.
A.3.5.2.4 standard solution W2. pipette 5mL ± 0.02mL standard solution W1 to 50mL volumetric flask, dilute with water to
Scale.
A.3.5.3 Preparation of test solution
A.3.5.3.1 Test solution S1. Weigh about 50mg samples, accurate to 0.0001g, set 10mL volumetric flask, dilute to the mark.
A.3.5.3.2 test solution S2. pipette 5mL ± 0.02mL test solution S1 to 50mL volumetric flask, diluted with water to the mark.
System suitability test A.3.5.4
By HPLC procedures warm-up, adjust the temperature and flow, to analyze the conditions and steady baseline. Repeat 3 times, respectively, injection
100μL into standard solution and standard solution W1 W2, β- isomer, alitame and alanine amides such as approximate retention time
Table A.2. The coefficient of variation of the peak area (100 times standard deviation divided by the average peak area) should not exceed 2%.
Table A.2 approximate retention times of the components
Ingredient name Approximate retention times/min
β- isomer 6
Alitame 10
Alanine amide 15
Note. The retention time of approximately 15cm × 0.4cm column obtained. If you use other columns or different lengths should be adjusted in the mobile phase of acetonitrile
Ratio to obtain the retention time required.
A.3.5.5 Determination
The mobile phase was pumped into the column to baseline no longer drift. Standard solution and the test solution was analyzed under the system suitability test conditions.
Injection three times the standard working solution W1, β- isomers and calculate the average peak area alanine amide. Injection three times standard solution
W2, calculate the average peak area of alitame. Inject test solution three times S1, β- isomers and calculate the average peak area alanine amide.
Three times injection test solution S2, calculate the average peak area of alitame.
A.3.6 Calculation Results
Alitame content (dry basis) of the mass fraction w1, according to equation (A.1) Calculated.
w1 =
RA × WS × PS
RS × WA ×
100% (A.1)
Where.
RA --- test solution S2 detected peak response value;
WS --- alitame standard samples after subtracting the mass of water, in grams (g);
PS --- β- alanine amide isomer or purity standard sample,%;
Response value RS --- standard working solution W2 detected peak;
WA --- sample after subtracting the mass of water, in grams (g).
β- isomer (dry basis) of the mass fraction w2, according to equation (A.2) Calculated.
w2 =
RA × WS × PS × DF
RS × WA ×
100% (A.2)
Where.
RA --- test solution S1 detected peak response value;
--- The WS mass β- isomer or alanine amide standard sample of the standard sample of water was not removed, in grams (G);
PS --- β- isomer purity standard sample,%;
DF --- dilution factor, namely 0.003;
Response value RS --- standard working solution W1 detected peak;
WA --- water quality samples were not removed, in grams (g).
Alanine amide (dry basis) of the mass fraction w3, according to equation (A.3) Calculated.
w3 =
RA × WS × PS × DF
RS × WA ×
100% (A.3)
Where.
RA --- test solution S1 detected peak response value;
WS --- standard sample or standard sample quality alanine amide β- isomers of moisture is not removed, in grams (g);
PS --- β- isomer purity standard sample,%;
DF --- dilution factor, namely 0.003;
Response value RS --- standard working solution W1 detected peak;
WA --- water quality samples were not removed, in grams (g).
A.4 Determination of specific rotation αm (25 ℃, D) of
A.4.1 Weigh 10g sample to the nearest 0.001g, dissolved in water and transferred to a 1000mL volumetric flask, dilute to the mark, shake,
Measurement temperature of 25 ℃ ± 0.5 ℃.
Specific rotation αm (25 ℃, D), to "(°) · dm2 · kg-1" meter, according to equation (A.4) Calculated.
αm (25 ℃, D) =
l × ρα
(A.4)
Where.
α --- measured rotation angle in degrees (°);
L --- optical tube length, measured in decimeters (dm);
Ρα --- mass concentration of the effective component in solution, in grams per milliliter (g/mL).
A.4.2 Other press GB/T 613 performed.
Appendix B
Alitame standard infrared spectra
Food additives alitame standard infrared spectrum is shown in Figure B.1.
Figure B.1 alitame standard infrared spectra
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