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GB 1886.187-2016 English PDF

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GB 1886.187-2016: Food additive -- Sorbitol solution
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Basic data

Standard ID GB 1886.187-2016 (GB1886.187-2016)
Description (Translated English) Food additive -- Sorbitol solution
Sector / Industry National Standard
Classification of Chinese Standard X40
Word Count Estimation 14,189
Date of Issue 2016-08-31
Date of Implementation 2017-01-01
Older Standard (superseded by this standard) GB 7658-2005; GB 29219-2012
Regulation (derived from) Announcement of the State Administration of Public Health and Family Planning 2016 No.11
Issuing agency(ies) National Health and Family Planning Commission of the People's Republic of China, State Food and Drug Administration

GB 1886.187-2016: Food additive -- Sorbitol solution

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(Food safety national standard - Food additive - Sorbitol and sorbitol) National Standards of People's Republic of China National Food Safety Standard Food additives Sorbitol Sorbitol solution Issued on.2016-08-31 2017-01-01 implementation People's Republic of China National Health and Family Planning Commission released

Foreword

This standard replaces GB 29219-2012 "national food safety standards for food additives sorbitol" and GB 7658-2005 "food Additives sorbitol solution. " This standard compared with GB 29219-2012, GB 7658-2005, the main changes are as follows. --- Standard name was changed to "national food safety standards for food additives sorbitol and sorbitol solution"; --- Modify the scope; --- Modify the sensory requirements; --- Modified solid indicators sorbitol solution, sorbitol total sugar index; --- Remove the physical and chemical indicators of arsenic, heavy metals, pH, relative density index; --- Adds Bennett titration sugar; --- Modify part detection method. National Food Safety Standard Food additives Sorbitol Sorbitol solution

1 Scope

This standard applies to milk or starch such as corn starch processing plants obtained by hydrolysis, refined into glucose, the role of catalyst in After the hydrogenation reaction, and then after refining, the process of producing concentrated food additive sorbitol liquid and sorbitol solution then was concentrated and dried, Screening and other processes to prepare food additive sorbitol. 2 molecular formula, relative molecular mass and structural formula Formula 2.1 C6H14O6 2.2 formula 2.3 relative molecular mass 182.17 (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 index Sorbitol sorbitol solution Testing method Colorless, transparent white color The state of powder, flakes or granules, hygroscopic viscous liquid Take appropriate samples, under natural light, observe the color and status 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 project index Sorbitol sorbitol solution Testing method Sorbitol content, w /% ≥ 91.0 (dry basis) 50.0 Appendix A A.3 Water, w /% ≤ 1.5 31.0 Sorbitol. GB 5009.3 Method II or IV Law (Arbitration Act) Sorbitol solution. GB/T 6284a or GB 5009.3 The fourth method (Arbitration Act) Reducing sugar (glucose), w /% ≤ 0.3 0.21 Appendix A A.4 Total sugar (glucose), w /% ≤ 4.4 8.0 Appendix A A.5 Residue on ignition, w /% ≤ 0.1 0.1 Appendix A A.6 Sulfate (SO4 meter)/(mg/kg) ≤ 100 50 Appendix A A.7 Chloride (based on Cl)/(mg/kg) ≤ 50 10 Appendix A A.8 Nickel (Ni)/(mg/kg) ≤ 2.0 2.0 GB 5009.138 Lead (Pb)/(mg/kg) ≤ 1.0 1.0 GB 5009.12 Weigh about 1g a sample, accurate to 0.0002g, ± at 130 ℃ 2 ℃ drying 4h.

Appendix A

Testing method A.1 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 regulations. test The standard solution titration experiments, impurity measurement standard solution, preparations and products, did not indicate when the other requirements, according to GB/T 601 used, GB/T 602 and GB/T 603 provisions 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 In measuring the content of sorbitol in the test, the sample solution chromatogram peak retention time of the standard solution in the chromatogram peak retention Retention time consistent. A.3 Determination of Sorbitol Content A.3.1 Method summary By high performance liquid chromatography, under the selected operating conditions, using water as the mobile phase through the column so that the separation of the components in the sample solution with Refractive Index Detector to detect, by the data processing system of recording and processing the chromatographic signal. A.3.2 Reagents and materials A.3.2.1 Water. in line with GB/T 6682 water level. A.3.2.2 sorbitol Standard sample. mass fraction ≥98.0%. A.3.3 Instruments and Equipment High performance liquid chromatograph. equipped with a differential refractive index detector. A.3.4 reference chromatographic conditions A.3.4.1 Mobile phase. water (A.3.2.1), using 0.22μm filter membrane, ultrasound degassing spare. A.3.4.2 Column. calcium type strong acid cation exchange resin as a filler dedicated to sugar and sugar alcohols analytical column, column length 300mm, column An inner diameter of 7.8mm, or other equivalent column. A.3.4.3 Column temperature. 70 ℃ ~ 90 ℃, and controlling the temperature fluctuation should not exceed 1 ℃. A.3.4.4 mobile phase flow rate. 0.5mL/min ~ 1.0mL/min. A.3.4.5 Injection volume. 20μL. A.3.5 Analysis step A.3.5.1 Preparation of standard solutions Weigh 5.0g sorbitol standard sample, accurate to 0.0002g, in 100mL volumetric flask, dissolved in mobile phase, dilute to volume Volume, and mix. Chromatographic analysis before using 0.45μm microporous membrane filtration. A.3.5.2 Preparation of sample solution Weigh 5.0g sample, accurate to 0.0002g, in 100mL volumetric flask, dissolved in mobile phase, dilute to volume, mix, color Before spectral analysis with 0.45μm microporous membrane filtration. A.3.6 Determination A.3.6.1 external standard method (Arbitration Act) In reference A.3.4 chromatographic conditions, respectively, sample solution and standard solution were chromatographed recording standard solution obtained sorbitan mountain Sorbitol Au alcohol peak area peak area of the sample solution and As. A.3.6.2 area normalization method In A.3.4 reference chromatographic conditions, the sample solution was subjected to chromatographic analysis, recording each chromatographic peak area. According peak area to Area calculation sorbitol content of normalization. A.3.7 Calculation Results A.3.7.1 external standard method (Arbitration Act) Sorbitol content mass fraction w1, according to formula (A.1) Calculated. w1 = Au × ms × ws As × mu × 100% (A.1) Where. Peak area Au --- sample solution of sorbitol; Quality ms --- sorbitol standard sample in grams (g); ws --- standard sample sorbitol mass fraction,%; As --- peak area of standard solution of sorbitol; Quality mu --- sorbitol liquid sample, or dry mass of sorbitol sample in grams (g). The results parallel arithmetic mean of the measurement results shall prevail. Twice under the same condition of independent determination results obtained absolute difference Not more than 0.5%. A.3.7.2 area normalization method Sorbitol content mass fraction w1, according to equation (A.2) Calculated. w1 = Au Asum × 100% (A.2) Where. Peak area Au --- sample solution of sorbitol; --- In the sample solution as in ASUM total peak area of all peaks. The results parallel arithmetic mean of the measurement results shall prevail. Twice under the same condition of independent determination results obtained absolute difference Not more than 0.5%. A.4 reducing sugar (glucose) Determination A.4.1 Bennett titration A.4.1.1 Method summary Bennett reducing sugars in the sample reagent divalent copper ion reacts with the red cuprous oxide, cuprous oxide when iodine is oxidized, and Into divalent copper ions, the excess iodine with sodium thiosulfate, oxidation reaction consumption to calculate the iodine content of reducing sugar. A.4.1.2 Reagents and solutions A.4.1.2.1 hydrochloric acid solution. 1mol/L. Measure 84mL of hydrochloric acid (37%), dissolved dubbed 1000mL. A.4.1.2.2 iodine standard solution. c ( 2I2 ) = 0.04mol/L. Weigh 7.2g of potassium iodide and iodine 5.0762g dubbed 1000mL solution, Stored in a brown bottle (need to stand shake after use 24h). A.4.1.2.3 sodium thiosulfate standard titration solution. c (Na2S2O3) = 0.04mol/L. A.4.1.2.4 acetic acid solution. 5%. A.4.1.2.5 phenolphthalein indicator solution. 10g/L. A.4.1.2.6 starch indicator solution. 10g/L. A.4.1.2.7 Bennett reagents. 16g in 150mL of water was added copper sulfate (CuSO4 · 5H2O), stirring to dissolve, this is the solution A. in 650mL water, 150g of trisodium citrate was added successively, 130g of anhydrous sodium carbonate, 10g of sodium hydrogencarbonate, and dissolved by heating, to this solution B. The cooled solution A was mixed with solution B, dilute with water to 1000mL filtering, aging 24h after use. A.4.1.3 analysis step Weigh sorbitol sample 3.3g, weighed sorbitol liquid sample 5g, accurate to 0.001g, in 250mL conical flask, Benny Special reagent 20mL, add a few grains of glass beads, heating and controlling the temperature exactly inside 4min ± 0.25min boil and continue to boil 3min (accurate Timing) after rapid cooling with tap water. In the first conical flask was added 50mL of water plus acetic acid 50mL, accurate pipette iodine standard solution was added 20mL, add salt Acid solution 25mL, Shake the red precipitate is completely dissolved, the excess iodine back titration with sodium thiosulfate standard titration solution, towards the end (by the Dark brown pale green), add about 5 drops of starch indicator solution and continue titration until the color turned light blue as the end point. 5mL amount of water according to the above procedures blank test, recording body titration of sodium thiosulfate standard solution consumed in the blank test Volume V0. A.4.1.4 The results are shown Reducing sugar (glucose) mass fraction w2, according to equation (A.3) Calculated. w2 = V0-V1 () × c × 0.112 0.04 × m (A.3) Where. Volume V0 --- blank test consumption of sodium thiosulfate standard titration solution, in milliliters (mL); Volume V1 --- sample consumption of sodium thiosulfate standard titration solution, in milliliters (mL); C --- concentration of sodium thiosulfate standard titration solution, expressed in moles per liter (mol/L); 0.112 --- 0.04mol/L of iodine ( 2I2 ) Equivalent glucose 0.112g; M --- the quality of the sample, in grams (g). 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 0.01%. A.4.2 potassium permanganate titration (Arbitration Act) A.4.2.1 Method summary At a certain temperature, time and concentration of the heat conditions, reducing sugars in the sample by excess Fehling peroxide solution, the reaction of cuprous oxide The precipitate was cuprous oxide to ferric reduced to ferrous sulfate standard titration with potassium permanganate solution titration generated ferrous sulfate. The high manganese Potassium consumption standard titration solution, check potassium permanganate oxidation of copper - conversion of glucose to get glucose meter quality by calculated the sugar (Glucose) levels. A.4.2.2 Reagents and materials A.4.2.2.1 Fehling solution. A.4.2.2.2 ferric sulfate. 50g/L. Weigh 50g iron sulfate, dissolved in water was added after 200mL, 100mL sulfuric acid was added slowly, stirring Diluted to 1000mL water after cooling mix. A.4.2.2.3 standard potassium permanganate titration solution. c ( 5KMnO4 ) = 0.1mol/L. A.4.2.3 instruments and equipment Sand core crucible. filter plate aperture 5μm ~ 15μm (G4). A.4.2.4 analysis step A.4.2.4.1 Weigh 20g ~ 50g sample (determined based on the amount of sugar-containing sample weight), accurate to 0.0002g, containing a small amount has been placed Water 250mL Erlenmeyer flask. A.4.2.4.2 plus 40mL Fehling solution and a few glass beads, shake well. Placed on the heating furnace, control boiling in 4min, continue Boil 3min, rapidly cooled to room temperature, and immediately with sand core crucible vacuum filtration, repeatedly washed with warm water beaker and precipitate the filtrate was clear, Until the filtrate was not alkaline, discard the filtrate washed suction bottles. In the sand core crucible carve 3 plus 60mL solution of ferric sulfate, copper oxide Shen Fully dissolved precipitate, filtration, and washed with water several times the sand core crucible filtrate was collected. Titration with potassium permanganate standard solution titrate the filtrate to a reddish end. Record actual consumption of standard potassium permanganate titration solution volume V0. A.4.2.5 Calculation Results Conversions A.4.2.5.1 potassium permanganate standard titration solution volume Standard potassium permanganate titration solution [c ( 5 KMnO4 )] In terms of volume V1, in milliliters (mL), according to equation (A.4) Calculated. V1 = V0 × c1 0.1000 (A.4) Where. V0 --- consumption of potassium permanganate titration standard solution (A.4.2.2.3) volume in milliliters (mL); Concentration c1 --- potassium permanganate standard titration solution, expressed in moles per liter (mol/L); 0.1000 --- c ( 5 KMnO4 ) = Concentration 0.1000mol/L of potassium permanganate standard titration solution, expressed in moles per liter (Mol/L). Calculation A.4.2.5.2 reducing sugar (glucose) content Reducing sugar (glucose) mass fraction w3, according to equation (A.5) Calculated. w3 = m1 m × 1000 × 100% (A.5) Where. m1 --- According V1 (A.4.2.5.1) look-up table B.1 mass calculated value obtained glucose in milligrams (mg); M --- the quality of the sample, in grams (g); 1000 --- conversion factor. 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 0.008%. A.5 total sugar (glucose) Determination A.5.1 Method summary Under acidic conditions, oxidation of the sample Fehling solution heated at reflux for glycan monosaccharides produced by hydrolysis by excess, the reaction of an alkylene oxide Copper precipitation, cuprous oxide to ferric reduced to ferrous sulfate standard titration with potassium permanganate solution titration generated ferrous sulfate. The high manganese Potassium consumption standard titration solution, check potassium permanganate oxidation of copper - conversion of glucose to get glucose meter quality by calculated the total sugar (Glucose) levels. A.5.2 Reagents and materials A.5.2.1 sodium hydroxide solution. 400g/L. A.5.2.2 hydrochloric acid solution. 18100. A.5.2.3 Bromocresol green - methyl red indicator solution. A.5.3 Analysis step Weigh 20g ~ 50g sample (based on the total amount of sugar-containing determine the sample weight), accurate to 0.0002g, placed in 500mL conical grinding mouth bottle In; add approximately 80mL water 100mL hydrochloric acid solution, fitted with condenser was heated to reflux. Boiling start time, continue boiling 45min, after cooling, add Bromocresol green - methyl red indicator solution, and to the solution with sodium hydroxide solution pH of about 7 and transferred to 250mL or 500mL volumetric flask (according to Determine the amount of total sugar-containing flask of volume), diluted with water to the mark, shake well, pipetting 20.00mL, placed in 250mL conical flask. The following operation is the same A.4.2.4.2. A.5.4 Calculation Results A.5.4.1 c ( 5 KMnO4 ) = 0.1mol/L potassium permanganate standard titration solution in terms of volume V1 conversion with A.4.2.5.1. A.5.4.2 total sugar (glucose) mass fraction w4, according to equation (A.6) Calculated. w4 = m1 m × 1000 × (20/V2) × 100% (A.6) Where. m1 --- based on the quality V1 (A.4.2.5.1) look-up table B.1 give glucose in milligrams (mg); M --- the quality of the sample, in grams (g); 1000 --- quality conversion factor; 20.00mL sample solution 20 --- Pipette, expressed in milliliters (mL); --- V2 of the flask transferred volume in milliliters (mL). 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 0.08%. A.6 Determination of residue on ignition A.6.1 Analysis step Sample taken 2g ~ 5g, quality constant weight has been placed in a crucible, accurate to 0.0002g. Slowly on the electric ignition to completely carbonized, cold To room temperature, a sufficient amount of sulfuric acid wetting, low temperature sulfuric acid heated to steam out to do. Then transferred to a high temperature furnace at 800 ℃ ± 25 ℃ Burning to completely gray, and then weighed to constant mass. A.6.2 Calculation Results Burning residue mass fraction w5, according to equation (A.7) calculated as follows. w5 = m1-m0 m2-m0 × 100% (A.7) Where. After the mass m1 --- crucible and residue on ignition in grams (g); Mass m0 --- empty crucible in grams (g); Mass m2 --- crucible with the sample, in grams (g). The results parallel arithmetic mean of the measurement results shall prevail. Twice under the same condition of independent determination results obtained absolute difference Not more than 0.02%. A.7 Sulfate (SO4 meter) measurement A.7.1 Reagents and materials A.7.1.1 Potassium standard solution. Weigh accurately potassium sulfate 0.181g, dissolved in water and diluted to 1000mL volumetric flask, shake, That was (equivalent to 100μg per 1mL of SO4). A.7.1.2 hydrochloric acid solution. 1090. A.7.1.3 barium chloride solution. 250g/L. A.7.2 Instruments and Equipment A.7.2.1 analytical balance. a sense of the amount of 0.01g. A.7.2.2 Nessler colorimetric tube. 50mL. A.7.3 Analysis step Weigh 1g sample was placed Nessler colorimetric tube, dissolved in water to make into a 40mL, hydrochloric acid solution was added 2mL, shake, is the test solution. For sorbitol samples, take another one Nessler colorimetric tube, add potassium sulfate standard solution 1mL, add water to make into a 40mL, hydrochloric acid is added Solution 2mL, shake, is the control solution. For sorbitol liquid samples, take another one Nessler colorimetric tube, add potassium sulfate standard solution 0.5mL, add water to make into a 40mL, added Hydrochloric acid solution 2mL, shake, is the control solution. In the test solution and control solution were added barium chloride solution 5mL, diluted with water to 50mL, fully shaking, 10min, Set on the same black background, the axial observation, comparison cloudy generated. A.7.4 results found Turbidity test solution is less than the control solution, judged as qualified; as for the test solution turbidity is greater than the control solution, as unqualified. A.8 chloride (Cl) Determination A.8.1 Reagents and materials A.8.1.1 sodium stock standard solution. Weigh accurately chloride 0.165g, dissolved in water and diluted to 1000mL volumetric flask, shake Even as the stock solution. 1mL of this solution is equivalent to 100μg of Cl. A.8.1.2 sodium chloride standard solution. the precise amount of sodium chloride stock standard solution 10mL, 100mL placed volumetric flask, dilute with water to Mark and shake. 1mL of this solution is equivalent to 10μg Cl. This solution is using now. A.8.1.3 silver nitrate solution. c (AgNO3) = 0.1mol/L. A.8.1.4 nitric acid solution. 1090. A.8.2 Instruments and Equipment A.8.2.1 analytical balance. a sense of the amount of 0.01g. A.8.2.2 Nessler colorimetric tube. 50mL. A.8.3 Analysis step Weigh 1g sample was placed Nessler colorimetric tube, dissolved in water to make into a 25mL, plus nitrate solution 10mL, add water to make into approximately 40mL, Shake, that was the test solution. For sorbitol samples, take another one Nessler colorimetric tube, add 5mL sodium chloride standard solution, dissolved in water to make into a 25mL, again Plus nitric acid solution 10mL, add water to make into approximately 40mL, shake, is the control solution. For sorbitol liquid samples, take another one Nessler colorimetric tube, add 1mL sodium chloride standard solution, dissolved in water to make into a 25mL, Plus nitrate solution 10mL, add water to make into approximately 40mL, shake, is the control solution. In the test solution and control solution were added to the silver nitrate solution 1.0mL, diluted with water to 50mL, shake, placed in the dark 5min, set on a black background the same axial observed turbidity generated. A.8.4 results found Test solution turbidity in shallow control solution, judged as qualified; as for the test solution concentrated to turbidity control solution, as unqualified.

Appendix B

Cuprous oxide potassium permanganate - reducing sugar (glucose) in terms of Potassium permanganate oxidation of copper - in terms of glucose in Table B.1. Table B.1 potassium permanganate oxidation of copper - in terms of glucose c ( 5 KMnO4 ) = 0.1000mol/L permanganate Potassium Standard Solution / ML Oxyalkylene Copper quality / Mg glucose Quality/mg c ( 5 KMnO4 ) = 0.1000mol/L permanganate Potassium Standard Solution / ML Oxyalkylene Copper quality / Mg glucose Quality/mg c ( 5 KMnO4 ) = 0.1000mol/L permanganate Potassium Standard Solution / ML Oxyalkylene Copper quality / Mg glucose Quality/mg 2.0 12.7 6.5 4.7 29.8 14.8 7.4 46.9 23.6 2.1 13.3 6.7 4.8 30.4 15.2 7.5 47.6 24.0 2.2 14.0 7.0 4.9 31.1 15.5 7.6 48.2 24.2 2.3 14.6 7.3 5.0 31.7 15.7 7.7 48.8 24.5 2.4 15.2 7.6 5.1 32.2 16.0 7.8 49.5 25.0 2.5 15.9 8.0 5.2 33.0 16.4 7.9 50.1 25.2 2.6 16.5 8.2 5.3 34.2 16.7 8.0 50.8 25.5 2.7 17.1 8.5 5.4 34.9 17.0 8.1 51.4 26.0 2.8 17.8 8.9 5.5 35.5 17.3 8.2 52.0 26.2 2.9 18.4 9.2 5.6 36.1 17.6 8.3 52.7 26.6 3.0 19.0 9.5 5.7 36.8 17.9 8.4 53.3 27.0 3.1 19.6 9.8 5.8 37.4 18.3 8.5 53.9 27.2 3.2 20.3 10.0 5.9 37.7 18.6 8.6 54.6 27.6 3.3 20.9 10.2 6.0 38.1 19.0 8.7 55.2 28.0 3.4 21.5 10.5 6.1 38.7 19.3 8.8 55.8 28.2 3.5 22.2 10.9 6.2 39.3 19.6 8.9 56.5 28.6 3.6 22.8 11.2 6.3 40.0 19.9 9.0 57.1 29.0 3.7 23.4 11.5 6.4 40.6 20.2 9.1 57.7 29.2 3.8 24.1 11.9 6.5 41.2 20...

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