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GB 1886.73-2015 English PDF

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GB 1886.73-2015: National Food Safety Standard -- Food Additives -- Insoluble polyvinylpolypyrrolidone
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GB 1886.73-2015English279 Add to Cart 3 days [Need to translate] National Food Safety Standard -- Food Additives -- Insoluble polyvinylpolypyrrolidone Valid GB 1886.73-2015

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Basic data

Standard ID GB 1886.73-2015 (GB1886.73-2015)
Description (Translated English) National Food Safety Standard -- Food Additives -- Insoluble polyvinylpolypyrrolidone
Sector / Industry National Standard
Classification of Chinese Standard X40
Word Count Estimation 13,115
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, State Food and Drug Administration

GB 1886.73-2015: National Food Safety Standard -- Food Additives -- Insoluble polyvinylpolypyrrolidone


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(National food safety standards for food additives insoluble polyvinylpolypyrrolidone) National Standards of People's Republic of China National Food Safety Standard Food additives insoluble polyvinylpolypyrrolidone 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 additives insoluble polyvinylpolypyrrolidone

1 Scope

This standard applies to N- vinylpyrrolidone monomer as a raw material in the presence of a basic catalyst or N, N'- divinyl - Mi Pyrazolone as a crosslinking agent to generate a food additive insoluble polyvinylpolypyrrolidone. 2 molecular formula, structural formula Formula 2.1 (C6H9NO) n 2.2 formula

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 or similar white State hygroscopic white powder Take appropriate amount of the sample to the transparent glass tube, in natural light black paper backing Observed 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 Nitrogen content, w /% 11.0 ~ 12.8 Appendix A A.4 Free N- vinylpyrrolidone/(mg/kg) ≤ 10.0 A.5 Appendix A pH (1% suspension) 5-8 Appendix A A.6 Water solubles, w /% ≤ 1.5 Appendix A A.7 Residue on ignition, w /% ≤ 0.4 Appendix A A.8 Free N, N'- divinyl - imidazolidinone/(mg/kg) a ≤ 2.0 A.9 Appendix A Water, w /% ≤ 6.0 Appendix A A.10 Lead (Pb)/(mg/kg) ≤ 2.0 GB 5009.12 Zinc (Zn)/(mg/kg) ≤ 25.0 GB 5009.14 Only use a N, N'- divinyl - imidazolidinone as a crosslinking product testing the project.

Appendix A

Testing method A.1 Safety Tips Reagents toxic or corrosive, operator of this test method should be used with caution. As should be immediately washed with water splashed on the skin Wash, severe cases should be treated immediately. When using flammable, do not use open flame heating. A.2 General Provisions This standard reagents and water, did not indicate when the other requirements, refer to the three water analytical reagent and GB/T 6682 stipulated. Standard Solution tests required, the determination of impurities standard solution, the test method used in preparations and products, did not indicate when additional requirements are According to GB/T 601, the provisions of the preparation of GB/T 602 and GB/T 603, the test used in the solution, in the absence of explanation, refer to the water Solution. A.3 Identification Test A.3.1 Solubility Test 1.0g samples were taken, were added 10mL of water, 10 mL of 95% ethanol, 10mL ether, should not dissolve. A.3.2 fading reaction A.3.2.1 Reagents and materials A.3.2.1.1 iodine solution. c ( 2I2 ) = 0.1mol/L. A.3.2.1.2 starch indicator. 10g/L. A.3.2.2 analysis step Weigh about 1g sample was dissolved in 10mL water, shaking 30s, to prepare a suspension, was added 0.1mL iodine solution, shaken vigorously, then add 1mL starch indicator, shake vigorously, no blue produce. A.3.3 Infrared Spectroscopy A.3.3.1 Method summary Take insoluble polyvinylpolypyrrolidone and reference samples, respectively, with potassium bromide tablet, infrared spectral scanning, the two infrared Absorption spectra for comparison. A.3.3.2 Reagents and materials A.3.3.2.1 insoluble polyvinylpolypyrrolidone reference. A.3.3.2.2 potassium bromide (spectroscopically pure). A.3.3.3 instruments and equipment A.3.3.3.1 infrared spectrometer. A.3.3.3.2 tablet device. A.3.3.4 analysis step Were taken from about 1mg of insoluble polyvinylpolypyrrolidone and reference samples, and about 100mg of potassium bromide carried out in an agate mortar Grinding, until thoroughly mixed. Take a little of the mixture powder into the tablet mold, pressed into a transparent sheet (salt window) is carried out using a tablet test. A.3.3.5 results found Insoluble polyvinylpolypyrrolidone infrared absorption spectrum of the sample should be the reference infrared absorption spectrum at 4000cm-1 ~ Absorption peaks in the range of 400cm-1 are similar. Insoluble polyvinylpolypyrrolidone infrared absorption spectrum of the reference, see Appendix B. A.4 Determination of nitrogen content A.4.1 Method summary The sample with sulfuric acid and catalyst were hot, and the organic nitrogen into ammonium, alkali distillation, after absorption of free ammonia with boric acid to sulfuric acid droplets standard Fixed titration, the nitrogen content calculated based on the volume of sulfuric acid consumed. A.4.2 Reagents and materials A.4.2.1 30% hydrogen peroxide. A.4.2.2 sulfuric acid. A.4.2.3 sodium hydroxide solution. 400g/L. A.4.2.4 boric acid. 40g/L. A.4.2.5 sulfuric acid standard titration solution. c ( 2H2SO4 ) = 0.05mol/L. A.4.2.6 mixed indicator. 2 parts of methyl red ethanol solution (1g/L) and 1 part of methylene blue ethanol solution (1g/L), temporary use when mixing. A.4.2.7 mixture of potassium sulfate and copper sulfate. 10 parts of the potassium persulfate, and 1 part of copper sulfate, milled into a powder form. A.4.3 Instruments and Equipment Kjeldahl distillation apparatus. A.4.4 Analysis step Accurately weigh 0.1g sample, accurate to 0.1mg, placed in 100mL Kjeldahl flask, a mixture of copper sulfate and potassium sulfate 1.0g, Draw 7mL sulfuric acid was added slowly along the sides of the bottle, to adhere to the bottleneck residue into the bottom of the bottle, shake, and then along the sides of the bottle slowly adding 1mL 30% hydrogen peroxide plus side carefully shaking the flask, and then multiple times (usually 3 to 6 times) was added 30% hydrogen peroxide, per ImL (note Italy. digestion process should not add 30% hydrogen peroxide), heating digestion until the solution became clear and bright green. Heating was continued for 4h, cooled After slowly adding 20mL water, the digestion solution into the distillation flask, plus the amount of wash water Kjeldahl flask, together with the cleaning liquid into the distillation Flask. The distillation flask connected to a distillation apparatus, and the end of the condenser has been added 15mL boric acid solution and 3 drops of mixed indicator Erlenmeyer flask Connection, should not absorbing liquid outlet through a condenser, a dropping funnel was added 30mL sodium hydroxide solution to a distillation flask, funnel spin off Plug immediately heated distillation. Distillate was collected until after the absorption liquid color green, continue to collect, collect until about 80mL ~ 100mL, stop steaming Distillate. Absorbing liquid sulfuric acid standard titration solution titration to pink, recording the volume of sulfuric acid standard titration solution. Meanwhile blank experiment. A.4.5 Calculation Results Nitrogen content of the sample to the mass fraction w1 meter, according to equation (A.1) Calculated. w1 = (V1-V2) × c × M m × 1000 × 100% (A.1) Where. V1 --- sample consumption volume of sulfuric acid standard titration solution, in milliliters (mL); V2 --- blank sample consumption of sulfuric acid standard titration solution volume in milliliters (mL); C --- concentration of sulfuric acid standard titration solution, expressed in moles per liter (mol/L); --- The M molar mass of nitrogen in grams per mole (g/mol), [M (N) = 14]; M --- the quality of the sample, in grams (g); 1000 --- conversion factor. The results to three significant figures. The test results of the arithmetic mean of the parallel determination results shall prevail, twice under the same condition of independent determination results obtained absolute difference Not more than 10% of the arithmetic mean. Determination of free N- vinyl pyrrolidone A.5 A.5.1 Method summary Insoluble polyvinylpolypyrrolidone free of N- vinylpyrrolidone extracted with water. After standing over the membrane using UV detection with High performance liquid chromatograph or diode array detector, external standard. A.5.2 Reagents and materials A.5.2.1 Methanol. HPLC grade. A.5.2.2 acetonitrile. HPLC grade. A.5.2.3 water, GB/T 6682 specified in a water. A.5.2.4 needle nylon membrane, pore size 0.22μm, or equivalent pore water system filters. A.5.2.5 N- vinylpyrrolidone reference substance, the content of ≥99%. A.5.2.6 N- vinylpyrrolidone standard stock solution. Weigh accurately 0.05gN- vinylpyrrolidone reference to the nearest 0.1mg, dissolved in methanol and diluted to 100mL, shake. A.5.2.7 N- vinylpyrrolidone intermediate standard solution. lessons 1mLN- vinylpyrrolidone standard stock solution, dilute with mobile phase Diluted to 100mL, shake. A.5.2.8 N- vinylpyrrolidone using standard solution. lessons 5mLN- vinylpyrrolidone intermediate standard solution, dilute with mobile phase Diluted to 100mL, shake. A.5.3 Instruments and Equipment Equipped with a UV detector or diode array detector HPLC. A.5.4 Analysis step A.5.4.1 Sample Preparation Accurately weighed 1.25g sample, accurate to 0.1mg, into the conical flask, accurately added 50mL of water, cover and seal, vibration on a shaker Swing 60min, to stand. The supernatant was filtered through a membrane (A.5.2.4). A.5.4.2 Reference conditions Liquid Chromatography A.5.4.2.1 Column. C18 column, column length 250mm, inner diameter 4.6mm, particle size 5μm, or equivalent separation column. A.5.4.2.2 mobile phase. acetonitrile - water (1090). A.5.4.2.3 flow rate. 1mL/min. A.5.4.2.4 detection wavelength. 235nm. A.5.4.2.5 Injection volume. 20μL. A.5.4.3 Determination According to the sample, the content of the measured object, select the analyte concentration within the instrument response linear response range was measured as beyond the instrument Linear response range should be diluted. Under the above chromatographic conditions, N- vinylpyrrolidone reference retention time is about 12.85min, standard Retention time standard solution and the sample solution was measured deviation should be within ± 2.5%. Appendix C liquid chromatograph of Figure C.1. A.5.5 Calculation Results Sample free N- vinylpyrrolidone mass fraction w2, in milligrams per kilogram (mg/kg), according to equation (A.2) Calculated. w2 = Ai × c × V × 1000 As × m × 1000 (A.2) Where. --- AI in the sample solution of N- vinylpyrrolidone peak area; C --- N- vinylpyrrolidone concentration of the standard solution, in micrograms per milliliter (μg/mL); V --- volume of extract, in milliliters (mL); --- AS solution of N- vinylpyrrolidone standard peak area; m --- sample mass, in grams (g); 1000 --- conversion factor. The results to three significant figures. The test results of the arithmetic mean of the parallel determination results shall prevail, twice under the same condition of independent determination results obtained absolute difference Not more than 10% of the arithmetic mean. A.6 pH (1% suspension) were measured Weigh 1g sample accurate to 0.01g, into the 150mL beaker, add water 100mL, according to GB/T 9724 were measured. A.7 Determination of water soluble matter A.7.1 Analysis step Weigh 10g sample, accurate to 0.01g, placed in 400mL beaker, weighed 100mL water was added to the beaker, glass rod stir well, Use 5cm magnetic stir bar, and stirred on a magnetic stirrer 1h. Stand until most of the solids precipitated. Take the upper solution to transfer all Centrifuge tube (make sure filtrate reached 50mL above), 3500r/min centrifugal 30min, the supernatant was carried out by the membrane pore size of 0.45μm Filtration, filtration time in order to prevent obstruction, can be placed on a membrane pore size 3μm in 0.45μm membrane filtration speed is slow can be manually or machine Mechanically stirred solution of the film, but to prevent damage to the membrane. Pipette 50mL clear filtrate has been placed at 105 ℃ ~ 110 ℃ oven temperature 3h dried and weighed beaker or evaporating dish, evaporated to dryness in a water bath, then at 105 ℃ ~ 110 ℃ constant temperature drying oven 3h, weighing, Accurate to 0.1mg. A.7.2 Calculation Results Sample mass fraction of water solubles w3, according to equation (A.3) Calculated. w3 = (M1-m0) × 2 m × 100% (A.3) Where. m1 --- dry beaker or evaporating dish and the total mass of the residue, expressed in grams (g); Mass m0 --- beaker or evaporating dish in grams (g); 2 --- conversion factor; M --- the quality of the sample, in grams (g). The results to two decimal places. Take two parallel determination results of the arithmetic average of the measurement results, the results of parallel determination of the absolute difference is not more than 0.05%. A.8 Determination of residue on ignition A.8.1 Reagents and materials A.8.1.1 sulfuric acid. A.8.1.2 sulfuric acid solution. The amount of sulfuric acid 57mL, slowly inject the right amount of water, cooled to room temperature, diluted with water to 1000mL. A.8.2 Analysis step Accurately weigh 2g samples, accurate to 0.1mg, placed in a burned to constant weight porcelain crucible, adding an appropriate amount of sulfuric acid solution, wetting placed An electric furnace or a hot plate heated slowly, so that the sample is completely dry. Heating is continued till the complete carbonization, cooling, 0.5mL sulfuric acid wetting The residue was then heated, until the residual sulfuric acid and the sample is completely volatilized. The crucible was placed in a furnace at 800 ℃ ± 25 ℃ burning 15min Or more, remove the crucible is cooled to about 200 ℃, desiccator, cooled to room temperature, and weighed. Repeat ignition until constant weight. A.8.3 Calculation Results Burning residue mass fraction w4, according to equation (A.4) Calculated. w4 = m1-m0 m × 100% (A.4) Where. After the burning of the total mass m1 --- crucible and ash in grams (g); Mass m0 --- constant weight of the crucible, in grams (g); M --- the quality of the sample, in grams (g). The results to two significant figures. Take two parallel determination results of the arithmetic average of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.05%. A.9 free N, N'- divinyl - Determination imidazolidinone A.9.1 Method summary The sample was added as an internal standard n-heptane nitrile, acetone extract free N, N'- divinyl - imidazolidinone used with NPD The gas chromatography, internal standard. A.9.2 Reagents and materials A.9.2.1 acetone. A.9.2.2 n-heptane nitrile content of ≥99%. A.9.2.3 N, N'- divinyl - imidazolidinone reference substance, the content of ≥99%. A.9.2.4 internal standard solution. Weigh accurately 0.1g n-heptyl nitrile, accurate to 0.1mg, placed 1000mL volumetric flask, dilute to the mark with acetone Degree, shake. A.9.2.5 N, N'- divinyl - imidazolidinone standard stock solution. Weigh accurately 0.025gN, N'- divinyl - imidazolidinone, precise To 0.2mg, placed in 100mL volumetric flask, dissolved in acetone and diluted to the mark. A.9.2.6 N, N'- divinyl - imidazolidinone intermediate standard solution. lessons 2mL standard stock solution in 50mL volumetric flask, with prop Ketones diluted to the mark. A.9.2.7 N, N'- divinyl - imidazolidinone using standard solution. lessons 2mL intermediate standard solution in 25mL volumetric flask, and then Draw 1mL of internal standard solution was diluted with acetone to the mark. A.9.3 Instruments and Equipment NPD with a gas chromatograph. A.9.4 Analysis step A.9.4.1 Determination of the correction factor Take the use of standard solution (A.9.2.7) in accordance with the conditions A.9.4.3 injection analysis, determination of the correction factor. A.9.4.2 Sample Preparation Accurately weigh 2.5g sample, accurate to 0.2mg, placed in 100mL conical flask with stopper, followed by accurate internal standard solution is added 1mL (A.9.2.4) and 24mL acetone, stamped seal, on the multifunction oscillator shaking 4h. Take appropriate extract to 10mL centrifuge tube, to 3000r/min centrifugal 2min, the supernatant. A.9.4.3 GC reference conditions A.9.4.3.1 Column. cross-linked polyethylene glycol bonded stationary phase, column length 30m, an inner diameter of 0.32mm, thickness of 0.2μm or equivalent separation Column. A.9.4.3.2 temperature program. 60 ℃ 1min, to a temperature increasing rate of 10 ℃/min was raised to 230 ℃. A.9.4.3.3 Inlet temperature. 220 ℃. A.9.4.3.4 detector temperature. 250 ℃. A.9.4.3.5 Carrier gas. nitrogen gas, the purity of 99.999% or more; flow rate was 2.0mL/min. A.9.4.3.6 hydrogen flow rate. 3.0mL/min. A.9.4.3.7 air flow rate. 60mL/min. A.9.4.3.8 Injection volume. 2μL. A.9.4.3.9 split ratio of 5. 1. A.9.4.3.10 Injection mode. split. A.9.4.4 Determination According to the test sample, the content of the sample solution, the concentration of selected analytes within the instrument response of the linear response range was measured as super The linear response range of the instrument should be diluted. Under the above chromatographic conditions, N, N'- divinyl - imidazolidinone reference retention time of about As 9.92min, gas chromatogram see Appendix C in Figure C.2. A.9.5 Calculation Results A.9.5.1 relative correction factor f, according to equation (A.5) Calculated. f = ms × Ai mi × As (A.5) Where. ms --- N, N'- divinyl - quality imidazolidinone, in milligrams (mg); Ai --- internal standard peak area; Mi --- the quality of the internal standard, in milligrams (mg); As --- N, N'- divinyl - imidazolidinone peak area. A.9.5.2 sample free N, N'- divinyl - imidazolidinone mass fraction w5, in milligrams per kilogram (mg/kg), according to formula (A.6) Calculated. w5 = f × As × mi × 1000 Ai × m (A.6) Where. f --- relative correction factor; --- AS sample N, N'- divinyl - imidazolidinone peak area; mi --- sample added mass of the internal standard, in milligrams (mg); 1000 --- conversion factor; Ai --- add sample peak area of the internal standard; m --- test sample mass, in grams (g). The results to two significant figures. The test results of the arithmetic mean of the parallel determination results shall prevail, twice under the same condition of independent determination results obtained absolute difference Not more than 10% of the arithmetic mean. A.10 Determination of moisture Accurately weigh 0.1g sample, accurate to 0.1mg, according to GB/T 6283 Determination.

Appendix B

Insoluble polyvinylpolypyrrolidone standard infrared spectrum Insoluble polyvinylpolypyrrolidone the standard infrared spectrum shown in Figure B.1. Figure B.1 insoluble crospovidone standard infrared spectrum (KBr tablet)

Appendix C

Standard solution N- vinylpyrrolidone and N, N'- divinyl - imidazolidinone the chromatogram of the standard solution Liquid chromatograph C.1 N- vinylpyrrolidone standard solution N- vinylpyrrolidone HPLC standard solution is shown in Figure C.1. Figure C.1 N- vinylpyrrolidone liquid chromatogram of the standard solution C.2 N, N'- divinyl - imidazolidinone gas chromatogram of the standard solution N, N'- divinyl - imidazolidinone standard solution Gas chromatography is shown in Figure C.2. Explanation. 1 --- n-heptane nitrile (internal standard); 2 --- N, N'- divinyl - imidazolidinone. Figure C.2 N, N'- divinyl - imidazolidinone gas chromatogram of the standard solution

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