GB 29929-2013Food additive -- 2-acetylated starch phosphate (English PDF)

2.1 Raw materials

2.1.1 Raw materials

Food starch should be consistent with national standards or industry standards-related products.

2.1.2 Accessories

2.1.2.1 should meet the national standards or industry standards or the relevant provisions of the relevant requirements of the product.

2.1.2.2 acetylation reagent type and amount of one of the following requirements.

a) of acetic anhydride, not more than 8.0% by mass of dry starch;

b) vinyl acetate, dry starch is not more than 7.5% mass fraction.

2.1.2.3 phosphorylation reagent type. Three partial sodium, phosphorus oxychloride.

2.2 Sensory requirements

Sensory requirements shall comply with the requirements of Table 1.

Table 1 Sensory requirements

Project requires test methods Color white, white or light yellow Take 50 g sample in a clean white porcelain dish, under natural light, observation its color, state, smell the smell Status granular, flaked or without visible impurities Inherent odor product smell, no odor

2.3 Physical indicators

Physical and chemical indicators should be consistent with the provisions of Table 2.

Table 2. Physical and chemical indicators

Item Index Test Method Loss on drying, w /% Cereal starch <= 15.0 GB/T 12087 other monomers starch <= 18.0 Potato starch <= 21.0 Total arsenic (As)/(mg/kg) <= 0.5 GB/T 5009.11 Lead (Pb)/(mg/kg) <= 1.0 GB 5009.12 Sulfur dioxide/(mg/kg) <= 30 GB/T 22427.13 Acetyl/(g/100g) <= 2.5 Appendix A A.4 Vinyl acetate residue (only with vinyl acetate as an esterification Agent)/(mg/kg) <= 0.1 A.5 in Appendix A the phosphate (with P meter)/% Potato or wheat starch <= 0.14 GB/T 22427.11 Other raw materials <= 0.04 Appendix A Testing method A.1 Safety Tips Reagents The standard test methods used for toxic or corrosive, the operation should be careful! As splashed on the skin should stand that is rinsed with water, severe cases should be treated immediately.

A.2 General Provisions Unless otherwise indicated in the analysis using only recognized as analytical reagents and GB/T 6682 stipulated three water. Test Methods the standard titration solution, impurity measurement standard solution, preparations and products, did not indicate when the other requirements, according to GB/T 601, GB/T 602 and 603 of the regulations prepared GB/T ; the solution when the solvent is not specified, refer to the aqueous solution.

A.3 Identification Test A.3.1 microscopy Without pasting treatment retention acetylated di starch phosphate particle structure can be directly observed and verified starch particle shape through the microscope, Size and character. Under polarized light microscope, it can be observed the typical birefringence.

A.3.2 iodine staining 1 g of the sample was added 20 mL of water were suspended, several drops of iodine solution, the color should range from deep blue to reddish brown.

A.3.3 copper reduction A.3.3.1 formulated alkaline tartrate copper test solution A.3.3.1.1 Solution A. Copper Sulfate (CuSO4 · 5H2O) 34.66 g, should be no weathering or moisture absorption phenomenon, dissolved in water volume to 500 mL.

The solution was stored in a small sealed container.

A.3.3.1.2 Solution B. take potassium sodium tartrate (KNaC4H4O6 · 4H2O) 173 g sodium hydroxide 50 g, dissolved in water volume to 500 mL.

The solution was stored in a small container and alkali corrosion.

A.3.3.1.3 solutions A and B mixed in equal volumes, to obtain an alkaline tartrate copper test solution.

A.3.3.2 analysis step Weigh the sample 2.5 g, placed in a flask, 0.82 mol/L hydrochloric acid solution of 10 mL of water and 70 mL, mixing, boiling water bath Was refluxed for 3 h, cooled. Take 0.5 mL solution was cooled, added 5 mL hot alkaline copper tartrate solution, a large amount of red precipitate.

A.4 Determination of acetyl group A.4.1 principle of the method Starch contains acetyl groups under alkaline conditions (pH >=8.5) saponification easily, so with excess alkali to saponification, then drops hydrochloric acid standard Fixed base titration solution can be determined the rest of acetyl content.

A.4.2 Reagents and materials A.4.2.1 sodium hydroxide.

A.4.2.2 hydrochloric acid.

A.4.2.3 sodium hydroxide solution. c (NaOH) = 0.1 mol/L.

A.4.2.4 sodium hydroxide solution. c (NaOH) = 0.45 mol/L. Weigh 18 g of sodium hydroxide dissolved in 100 mL of carbon dioxide-free water in, shake, transferred to a 1000 mL volumetric flask, dilute to the mark with carbon dioxide-free water and shake.

A.4.2.5 hydrochloric acid standard titration solution. c (HCl) = 0.2 mol/L. Measure 18 mL of hydrochloric acid, into 1000 mL of water, shake well.

A.4.2.6 phenolphthalein indicator solution. 10 g/L.

A.4.3 Instruments and Equipment Mechanical oscillator.

A.4.4 Analysis step

Weigh 5 g samples, accurate to 0.001 g, placed in 250 mL conical flask, 50 mL of water and 3 drops of phenolphthalein indicator solution, mixed Uniformly with sodium hydroxide solution (A.4.2.3) titrated to reddish, then add 25.0 mL of sodium hydroxide solution (A.4.2.4), mechanical vibration Turbulent 30 min for saponification the oscillator.

Remove the stopper, rinse bottle with iodine bottle stopper and the bottle wall, which has been saponified with hydrochloric acid standard solution titration solution containing an excess of base Titration to the disappearance of the pink is the end, volume V1.

In 25.0 mL of sodium hydroxide solution (A.4.2.4) blank, with the volume of hydrochloric acid standard solution titration is V0.

A.4.5 Calculation Results Mass fraction w0 acetyl group, according to the formula (A.1) Calculated.

0 xx

xx-= m

McVVw (A.1)

Where.

V0-- hydrochloric acid standard titration solution volume consumed in the blank, in milliliters (mL);

Hydrochloric acid standard titration solution volume V1-- sample consumed in milliliters (mL);

C-- exact concentration of hydrochloric acid standard titration solution, expressed in moles per liter (mol/L);

Molar mass M-- acetyl group, units of grams per mole (g/mol) [M (C2H3O) = 43.03];

Quality m-- sample in grams (g);

1000-- conversion factor.

A.5 Determination of residual vinyl acetate A.5.1 Reagents and materials A.5.1.1 vinyl acetate.

A.5.1.2 starch. samples with the same plant-derived and non-modified starch.

A.5.2 Instruments and Equipment GC. recommended with a flame ionization detector chromatograph.

A.5.3 chromatographic columns and typical operating conditions A.5.3.1 Column. capillary column, 60m × 0.32mm (internal diameter), the filling (50% cyanopropyl) - methyl polysiloxane.

A.5.3.2 oven temperature. programming, 40 °C heat 5 min, with 10 °C/min heating rate to 180 °C, at 180 °C heat 5 min.

A.5.3.3 Inlet temperature.200 °C.

A.5.3.4 detector temperature. 250 °C.

A.5.3.5 nitrogen as carrier gas (1.3 mL/min).

Alternatively with equivalent separation columns and corresponding chromatographic conditions.

A.5.4 Analysis step

A.5.4.1 Preparation of standard solutions Weigh 150 mg of vinyl acetate, accurate to 0.1 mg, into 100 mL volumetric flask, dissolved in water and diluted to the mark. Take 1 mL with a good solution into a 10 mL volumetric flask and dilute to the mark. The 0.1 mL of the diluted solution was added to 4 g of starch and equipped with a septum Plug instrument-specific bottle, sealed. This solution contains 15 µg of vinyl acetate.

A 5.4.2 Determination Weigh 4 g samples, accurate to 0.001 g, placed with a septum plug the instrument-specific bottle, sealed. Each containing samples and standards Special solution bottle into the instrument, under A.5.3 chromatographic conditions, headspace sampling to obtain chromatograms, peak area based on two maps Product calculating sample vinyl acetate content of.

A.5.4.3 Calculation Results Vinyl acetate residue w1 in mg/kg according to formula (A.2) Calculated.

Acw x=. (A.2)

Where.

c-- standard solution of acetic acid concentration of vinyl acetate, in milligrams per kilogram (mg/kg);

1A - signal peak area of the sample vinyl acetate produced;

2A - signal peak area of standard solution of vinyl acetate produced.