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GB 1886.141-2016

Search Result of Chinese Standard: 'GB 1886.141-2016'
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GB 1886.141-2016English179 Add to Cart Days<=3 (Food safety national standard - Food additive - Ribose) Valid GB 1886.141-2016
GB 1886.141-2016Chinese15 Add to Cart <=1-day [PDF from Chinese Authority, or Standard Committee, or Publishing House]

Detail Information of GB 1886.141-2016; GB1886.141-2016
Description (Translated English): (Food safety national standard - Food additive - Ribose)
Sector / Industry: National Standard
Classification of Chinese Standard: X09
Word Count Estimation: 10,166
Date of Issue: 2016-08-31
Date of Implementation: 2017-01-01
Regulation (derived from): Announcement of the State Administration of Public Health and Family Planning 2016 No.11

GB 1886.141-2016
(Food safety national standard - Food additive - Ribose)
National Standards of People's Republic of China
National standards for food safety
Food additives d-ribose
2016-08-31 released
2017-01-01 Implementation
People's Republic of China
National Health and Family Planning Commission released
National standards for food safety
Food additives d-ribose
1 Scope
This standard applies to glucose as raw material by fermentation method of food additives d-ribose.
2 chemical name, molecular formula, structural formula and relative molecular mass
2.1 Chemical name
(3R, 4R, 5R) -5- (hydroxymethyl) tetrahydrofuran-2,3,4-triol
2.2 Molecular formula
2.3 Structural formula
2.4 Relative molecular mass
150.13 (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 to yellowish
State crystalline powder
Place the sample on a clean white paper and observe it visually
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
d-ribose content, w /% 97.0 to 103.0 Appendix A, A.2
Melting point/℃ 80.0 ~ 90.0 Appendix A A.3
Specific rotation (20 ° C) - 21.0 ° ~ -19.0 ° GB/T 14454.5a
Dry reduction, w /% ≤ 2.0 Appendix A A.4
Burning residue, w /% ≤ 0.2 Appendix A A.5
Solution Transmittance /% ≥ 95.0 Appendix A A.6
Lead (Pb)/(mg/kg) ≤ 0.1 GB 5009.12 or GB 5009.75
Arsenic (As)/(mg/kg) ≤ 1.0 GB 5009.11 or GB 5009.76
a sample concentration. 4% (mass fraction) aqueous solution.
3.3 Microbial limits
Microbiological limits should be in accordance with Table 3.
Table 3 Microbial limits
Project limit test method
Total number of colonies/(CFU/g) ≤ 100 GB 4789.2
Mold, yeast/(CFU/g) ≤ 100 GB 4789.15
Escherichia coli/(CFU/g) ≤ 10 GB 4789.3
Salmonella/25g should not be detected GB 4789.4
Appendix A
Testing method
A.1 General provisions
The reagents and water used in this standard, when not specified in other requirements, refer to the analysis of pure reagents and GB/T 6682 provides three levels of water. test
The standard solution, impurity standard solution, preparation and article used in the test shall be classified according to GB/T 601, GB/T 602 and
GB/T 603. The solution used in the experiment, when not specified with the preparation of the solvent, refers to the aqueous solution.
A.2 Determination of d-ribose content
A.2.1 Methodological Summary
A chromatographic method was used to separate the specified mobile phase into a column packed with a filler by means of a high pressure infusion pump.
The injected sample is brought into the column by the mobile phase. The components are separated in the column and enter the detector in turn, either by the integrator or the data processing system
Record and process chromatographic signals.
A.2.2 Instruments and equipment
A.2.2.1 High performance liquid chromatograph.
A.2.2.2 ShodexKS-801 or other equivalent column.
A.2.2.3 10 μL dosing ring.
A.2.2.4 Electronic analytical balance (one ten thousandth).
A.2.3 Analysis requirements
A.2.3.1 Related Impurities. The main peak of the arabinose and d-ribose main peak to achieve complete separation.
A.2.3.2 Identification. Record the chromatogram, the retention time of the main peak of the reference solution and the retention time of the main peak of the sample solution
Should be consistent.
A.2.3.3 System adaptability. separation degree ≥ 1.2, relative standard deviation ≤ 0.5%, symmetry factor ≤ 1.3, theoretical plate number ≥ 2500.
A.2.4 Chromatographic conditions
A.2.4.1 Flow rate. 1.0 mL/min.
A.2.4.2 Column temperature. 80 ° C.
A.2.4.3 Detector temperature. 40 ° C.
A.2.4.4 Detector. Refractive detector.
A.2.4.5 Injection volume. 10 μL.
A.2.4.6 Run time. 15min.
A.2.4.7 Mobile phase. water.
A.2.5 Preparation of the solution
A.2.5.1 Preparation of mobile phase solution
Using chromatographic grade distilled water, the mobile phase was filtered with 0.45μm aqueous filter and ultrasonically 15min.
A.2.5.2 Preparation of impurity solutions
Accurately weigh 5 mg of arabinose in a 25 mL volumetric flask, dilute with 2% d-ribose solution and set the volume to a scale.
A.2.5.3 Contrast liquid
Accurately weighed three copies of the reference substance 0.5g (accurate to 0.0002g) placed in a 25mL volumetric flask, dissolved with mobile phase and constant volume
Degree, shake to be used.
A.2.5.4 Sample solution
Accurately weighed the two samples of the 0.5g (accurate to 0.0002g) placed in a 25mL volumetric flask, dissolved with mobile phase and fixed to the scale,
Shake up stand-by.
The sample and reference solution need to be filtered through a 0.45μm water phase filter and injected.
A.2.6 Analysis steps
A.2.6.1 System adaptability
Press the liquid chromatograph to test the operating procedures, open the instrument and make the instrument to a steady state, the first into a needle (quantitative ring 10μL) related
Impurities (arabinose) solution requires arabinose separation of ≥1.2, d-ribose main peak symmetry factor ≤ 1.3, d-ribose main peak theory
The number of plates ≥ 2500 to verify the main peak before the relevant impurities and d - ribose peak to achieve complete separation. After a needle blank, to verify the main peak
Before the relevant impurities no residual peaks. Finally, the three reference solutions were sequentially pipetted with the same volume of syringe (chromatographic
10μL), each reference substance were two needles, a total of six knots, respectively, to calculate the correction factor f1 ~ f6, using the correction factor according to formula (A.1) calculated
RSD ≤ 0.5%.
Relative standard deviation RSD, calculated according to formula (A.1).
i = 1
fi-􀭺 f
× 100% (A.1)
fi - i-th needle reference to the work of the correction factor, is the corresponding work reference weight and area ratio;
􀭺 f --- the average correction factor for the work reference;
n --- continuous take n needle work reference correction factor, n ≥ 6.
A.2.6.2 Determination
According to the preparation of the sample solution, on the basis of the system adaptability verification, the sample solution is used to clean the syringe and the injector,
The solution was injected into the chromatogram (10 μL of the loop) in the same manner, and each sample was mixed in two directions, and finally,
The corresponding solution is drift, the specific injection according to Table A.1 injection order.
Table A.1 Injection sequence
No. Name Injection number Injection volume
1 impurity solution 1 10 μL
2 blank solution 1 10 μL
3 Control solution 1 2 10 μL
4 Control solution 2 2 10 μL
Table A.1 (continued)
No. Name Injection number Injection volume
5 Control solution 3 2 10 μL
6 Sample solution 1 2 10 μL
7 Sample solution 2 2 10 μL
8 is different from the last two bottles of the control solution 2 10 μL
Note 1. When only a batch of samples, after the end of the batch after the end of the needle to enter the two needle No. 8 reference substance, the two goods in front of the sample with the four
For the calculation of the goods together, f RSD ≤ 0.5%.
Note 2. When there are multiple batches of samples, each batch of samples from the number 8 required to enter the 2-pin reference solution, the sample before the last 6-pin control solution correction
The average of the factors involved in the calculation of the sample results, f RSD ≤ 0.5%.
Note 3. Each batch of inspection records must be accompanied by all the parameters of the map, the map should have a number, the map must have a signature.
According to the external standard method to calculate the peak area.
The calibration factor fi of the reference substance is calculated according to formula (A.2)
fi =
M --- the quality of the reference substance, in grams (g);
S --- the peak area of the main peak of the reference substance.
The average correction factor for the reference substance is calculated according to equation (A.3).
􀭺f =
f1 f6
f1 ~ f6 --- correction factor for reference substance.
d-ribose content of the mass fraction w1, according to formula (A.4) calculation.
w1 =
S × P × 􀭺 f
M × (1 - w2) ×
100% (A.4)
S --- the main peak area of the sample;
P - content of reference substance,%;
􀭺 f --- the average correction factor for the reference substance;
M --- the quality of the sample, in grams (g);
w2 --- dry weight reduction of sample content,%.
A.2.7 Precautions
A.2.7.1 Pressure gauge No pressure display or pressure fluctuation can not be analyzed, should check whether the bubble in the pump has been excluded, the connection at or
Leakage, troubleshooting can be carried out before the operation.
A.2.7.2 There should be no dead volume connection between the column and the injector and its outlet end and the detector, so as to avoid sample diffusion.
A.2.7.3 Before applying the column, apply the mobile phase to full flush balance.
A.2.7.4 When the new column is contaminated with a suitable solvent, the outlet end should be disengaged from the detector to avoid contamination.
A.3 Melting point determination method
A.3.1 Methodological Summary
Material at an atmospheric pressure, from the solid state into a liquid to achieve equilibrium when the temperature, or melting at the same time the decomposition temperature, or in the melting
The temperature range that is experienced when it is initially melted to full melting.
A.3.2 Instruments and equipment
A.3.2.1 Visual melting point instrument. Accuracy of 0.1 ℃, range 0 ℃ ~ 280 ℃.
A.3.2.2 Capillary. Made of neutral hard glass, one end sealed, inner diameter 0.9mm ~ 1.1mm, wall thickness 0.10mm ~ 0.15mm, length
About 150mm.
A.3.2.3 Glass tube. Φ10mm × 800mm.
A.3.2.4 Agate or vitreous mortar. Φ60mm.
A.3.3 Analysis steps
A.3.3.1 The sample after the study was placed in a vacuum oven at -0.1 MPa 50 ℃ ± 2 ℃ (placed in place of phosphorus pentoxide) for 3 hours,
Immediately after removal, into a clean and dry capillary, take a Φ10mm × 800mm clean and dry glass tube, upright in the glass
, The capillary of the sample is placed in the upper end of the glass tube, allowing it to fall freely, repeated several times until the sample height in the capillary is compared
Accurately tightened to 3mm, the other end of the capillary sealed with vacuum grease to be measured.
A.3.3.2 set the melting point of the melting point of 70 ℃, the heating rate of 1.5 ℃/min, until the instrument reaches the starting temperature will be installed after the sample
Of the capillary into the sample cell to determine the direct visual record of the initial melting and final melting data, parallel determination of 3 times, 3 times between the results shall not exceed
0.2 ° C, whichever is the arithmetic mean, as the result of the analysis.
A.4 Determination of dry reduction
A.4.1 Methodological Summary
The temperature is below 100 ° C (including 100 ° C) and the pressure is below 2.76 kPa and dried under reduced pressure in the presence of phosphorus pentoxide
Box or vacuum dryer to dry the sample to constant weight.
A.4.2 Instruments and equipment
A.4.2.1 Electronic analytical balance (one ten thousandth).
A.4.2.2 Vacuum drying oven.
A.4.2.3 Rotary vane vacuum pump.
A.4.2.4 Flat weighing bottle.
A.4.3 Analysis steps
Accurately weighed 1.0g (accurate to 0.0002g) sample, tiled in the -0.1MPa 50 ℃ ± 2 ℃ under the conditions of drying to constant weight of the flat
Shaped sample bottle (specimen thickness can not exceed 5mm), and then the sample into the -0.1MPa 50 ℃ ± 2 ℃ filled with the amount of phosphorus pentoxide
As a desiccant in a vacuum oven and evacuated (vacuum pressure maintained at -0.1 MPa ± 0.05 MPa), kept dry for 3 h,
Cooler, cool to room temperature, accurately weighed. Continue drying under specified conditions for 1 h until the difference between the two after drying is less than the difference
A.4.4 Calculation of results
The mass fraction w2 of the drying reduction is calculated according to the formula (A.5)
w2 =
m1-m0 ×
100% (A.5)
m1 --- the quality of the sample and weighing bottle before drying, in grams (g);
m2 --- the quality of the dried sample and weighing bottle, in grams (g);
m0 --- Weigh the quality of the bottle, in grams (g).
A.4.5 Precautions
A.4.5.1 Decompression drying should use a single glass lid weighing bottle. If the glass cover for the double hollow, decompression, weighing the bottle should not be placed
Decompression drying oven, should be placed in another ordinary dryer.
A.4.5.2 The inside of the decompression dryer shall be negative. Before opening, keep the inlet valve slowly and let the dry air enter and avoid the blown
A.4.5.3 The weighing bottle containing the sample should be as close as possible to the temperature meter in order to avoid temperature error due to uneven temperature inside the tank.
A.5 Determination of burning residue
A.5.1 Methodological Summary
After the sample is added by adding sulfuric acid, burning to destroy the organic matter, generate sulfuric acid ash, said the residue weight, calculate the sample burning residue
The amount of.
A.5.2 Reagents and materials
A.5.2.1 Sulfuric acid.
A.5.2.2 discoloration silica gel.
A.5.3 Instruments and equipment
A.5.3.1 porcelain crucible.
A.5.3.2 High temperature furnace (range 0 ℃ ~ 900 ℃).
A.5.3.3 Crucible pliers.
A.5.3.4 Electronic analytical balance (one ten thousandth).
A.5.3.5 Adjustable electric furnace.
A.5.3.6 1mL pipette.
A.5.3.7 Dryers.
A.5.4 Analysis steps
Accurately weighed 1.0g (accurate to 0.0002g) sample, set in 500 ℃ ~ 600 ℃ high temperature furnace to the constant weight of the crucible. Electricity
The furnace slowly heated to the sample to the whole carbonization of the sample was black, and no longer smoke, let cool to room temperature. And 0.5 mL to 1 mL of sulfuric acid was added dropwise to obtain carbonization
All the heat, continue to heat in the electric furnace to remove the sulfuric acid vapor, white smoke completely disappeared (the above operation should be carried out in the fume hood). Will crucible
In the high-temperature furnace, the crucible cover is obliquely capped on the crucible, and the sample is completely ashes in the high-temperature furnace at 500 ℃ ~ 600 ℃ for about 3h. Move away
(About 1h), accurately weighed, if not qualified, then re-add sulfuric acid infiltration, repeat the previous steps for heating and burning
Burn, accurately weighed. In the prescribed conditions continue to burn for 30min, until the two consecutive burning after weighing the difference is less than 0.3mg.
A.5.5 Calculation of results
The mass fraction w3 of the burning residue is calculated according to formula (A.6)
w3 =
m1-m0 ×
100% (A.6)
m2 - the mass of the residue and crucible after constant weight, in grams (g);
m0 --- constant weight crucible after the mass, in grams (g);
m1 --- constant weight after the crucible and the quality of the sample, in grams (g).
A.5.6 Precautions
A.5.6.1 The previous operation of carbonization and ashing shall be carried out in a fume hood. The sample is placed in a high-temperature furnace before being completely carbonized and removed by sulfuric acid
Gas, if necessary, high temperature furnace should be installed exhaust pipe.
A.5.6.2 Crucibles shall be coded and the lid and the crucible shall be coded. From the high temperature furnace when the temperature, the order, in the dryer
Of the cooling time and the order of weighing, should be consistent before and after the same drying inside the crucible should not be placed more than 4, or difficult to reach
Constant weight.
A.5.6.3 After the crucible is cooled, it is easy to form a negative pressure in the dryer, and the dryer should be carefully opened to avoid blowing the light residue in the crucible.
A.5.6.4 If the residue is left for heavy metal inspection, the amount of the sample should be 1.0g, the burning temperature should be controlled at 500 ℃ ~
600 ° C.
A.5.6.5 When switching the door, care should be taken not to damage the high quality refractory insulation.
A.6 Determination of transmittance of solution
A.6.1 Methodological summary
By measuring the measured material in a specific wavelength or a certain range of absorption, the material qualitative or quantitative analysis method.
The ratio of the transmitted light flux passing through the sample solution to the incident light flux to the sample solution is expressed as a percentage.
A.6.2 Instruments and equipment
A.6.2.1 Spectrophotometer.
A.6.2.2 Capacity bottles.
A.6.2.3 Electronic analytical balance (ten thousandths).
A.6.3 Analysis steps
Weigh 5.0 g of the sample, placed in a 100 mL volumetric flask, dissolved in water and diluted to the mark. The sample solution was rinsed with 1 cm of quartz
And the sample solution was slowly injected into a 1 cm quartz absorption cell and the light transmittance was measured at a wavelength of 430 nm by spectrophotometry.
Repeat read 3 times, take the average value for the measured value.
A.6.4 Precautions
A.6.4.1 When taking the absorption cell, the fingers take the sides of the glass surface. The use of quartz absorption pool should be clean.
A.6.4.2 should be used before the first pairing test, that is used to hold the sample solution, the reference solution and blank solution of the absorption tank, when the same solvent
, The light transmittance of the absorption cell at the specified wavelength measurement, such as the difference in light transmittance of 0.3% or less, can be used for pairing, otherwise it should be corrected.
A.6.4.3 When the sample solution is contained, rinse the sample solution twice to three times to ensure that the sample solution is kept constant. The sample solution is filled with the absorption cell
The volume of four-fifths is limited.
A.6.4.4 When the absorption cell is placed in the sample chamber, note that the orientation and position should be the same.
Related standard:   GB 1886.127-2016
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