GB 29931-2013Food additive -- Hydroxypropyl 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 phosphorylation reagent type and amount. phosphorus oxychloride or sodium trimetaphosphate, the amount does not exceed the dry starch content of 0.1%.

2.1.2.3 etherifying agent type and amount. propylene oxide, no more than dry starch content of 10%.

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 plate in 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 the phosphate (As P) /% Potato or wheat starch <= 0.14 GB/T 22427.11 Other raw materials <= 0.04 Hydroxypropyl/(g/100g) <= 7.0 Appendix A A.4 Chloropropanol/(mg/kg) <= 1.0 A.5 in Appendix A 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 Gelatinization process without holding grain structure hydroxypropyl distarch phosphate, can be directly observed through a microscope to identify the shape of the starch granules, big Small and features. Under polarized light microscope, it can be observed the typical birefringence.

A.3.2 iodine staining the sample was 1 g 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 back Stream 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 hydroxypropyl A.4.1 principle of the method Hydroxypropyl distarch phosphate of propylene glycol in sulfuric acid, and then further dewatered propylene glycol propionaldehyde and propylene glycol, both dehydrated product it was to generate a purple complex with ninhydrin in sulfuric acid medium. Spectrophotometric measurement of absorbance at 590 nm at a concentration range of 5 mg ~ 50 mg, in line with Lambert - Beer law.

A.4.2 Reagents and materials A.4.2.1 sulfuric acid.

A.4.2.2 ninhydrin.

A.4.2.3 sodium bisulfite.

A.4.2.4 ninhydrin solution. ninhydrin dissolved in 5% sodium bisulfite solution to give a 3% solution of ninhydrin.

A.4.2.5 sulfuric acid solution. c ( H2SO4) = 1.0 mol/L.

A.4.2.6 1,2- propanediol.

A.4.2.7 Starch. not with the same modified starch of vegetable origin.

A.4.3 Instruments and Equipment Spectrophotometer.

A.4.4 Analysis step

A.4.4.1 preparation of standard solution Preparation of standard solutions of 1,2-propanediol 1.00 mg/mL, and Pipette 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL, 5.00 mL this standard solution to 100 mL volumetric flask, dilute to the mark, to give concentrations of 10 µg/mL, 20 µg/mL, 30 µg/mL, Standard solution 40 µg/mL and 50 µg/mL of.

A.4.4.2 preparation of the sample solution Weigh 50 mg ~ 100 mg sample to the nearest 0.1 mg, into 100 mL volumetric flask, add sulfuric acid solution 25 mL. In a boiling water bath Heated to dissolve the sample, after cooling diluted with water to 100 mL. If necessary, further diluted with 100 mL ensure that each contained hydroxypropyl Group does not exceed 4 mg, and then diluted in the same proportion blank starch.

A.4.4.3 Determination Take five standard solution of 1 mL, were transferred to 25 mL stoppered graduated test tube inside the tube was placed in cold water, sulfuric acid were added dropwise 8 mL, After mixing tube in a boiling water bath for accurate heating within 3 min, the tube was immediately transferred to a cold water bath to cool. Along the tube wall was carefully added copper ninhydrin solution Liquid 0.6 mL, shaking immediately, keep the 100 min at 25 °C water bath. With sulfuric acid to adjust the volume of each test tube to 25 mL, inverted test tube number Times to mix (do not shake). Now part of the solution transferred to the spectrophotometer 1 cm colorimetric pool and let stand for 5 min, measured at 590 nm at Reference absorbance standard curve.

Draw sample solution 1 mL, transferred to 25 mL with stopper in the test tube scale, subsequent operations in accordance with the standard solution measurement process, in order to precipitate Pink blank solution as reference, measured absorbance values.

A.4.5 Calculation Results Hydroxypropyl mass fraction w0, according to formula (A.1) Calculated.

7763.0

w (A.1)

Where.

C-- sample solution read from the standard curve in propylene glycol content in micrograms per milliliter (µg/mL);

0.7763-- glycol content into hydroxypropyl content conversion coefficient;

The final volume dilution f-- sample after milliliters (mL);

Quality m-- sample, in milligrams (mg);

1000-- conversion factor.

Determination A.5 chloropropanols A.5.1 Reagents and materials A.5.1.1 anhydrous ether.

A.5.1.2 Chloropropanol. containing 75% 1-chloro-2-propanol and 25% of 2-chloro-1-propanol.

A.5.1.3 silica. 250 µm ~ 150 µm.

A.5.1.4 sulfuric acid.

A.5.1.5 sodium hydroxide.

A.5.1.6 over anhydrous sodium sulfate.

A.5.1.7 sulfuric acid solution. c ( H2SO4) = 2 mol/L. Measure 60 mL of sulfuric acid, slowly into 1000 mL of water, cooling and shake.

A.5.1.8 sodium hydroxide solution. 25%. Weigh 25 g of sodium hydroxide dissolved in 75 mL of water.

A.5.1.9 waxy maize starch. modified waxy maize starch without treatment.

A.5.2 Instruments and Equipment A.5.2.1 GC. recommended with a flame ionization detector double-column chromatography.

A.5.2.2 pressure bottle.200 mL pressure bottle with a neoprene mat, glass stopper.

A.5.3 chromatographic columns and typical operating conditions A.5.3.1 Column. capillary column, 30m × 0.32mm (internal diameter), for the filling of polyethylene glycol 20M (PEG20M).

A.5.3.2 oven temperature. programming, 50 °C incubated 5min, at a rate of 10 °C/min raised to 220 °C, insulation 2min.

A.5.3.3 Inlet temperature. 250 °C.

A.5.3.4 detector temperature. 250 °C.

A.5.3.5 combustion gas is hydrogen (47mL/min), the combustion assisting gas is air (400mL/min), the compensation gas is nitrogen gas (30mL/min).

A.5.3.6 carrier gas nitrogen (25mL/min), split ratio 2. 1.

Alternatively with equivalent separation columns and corresponding chromatographic conditions.

A.5.4 Analysis step

A.5.4.1 Preparation of standard solution chloropropanols Using 10µL syringe take 5µL chloropropanols. Accurately weigh 500mL capacity and quality to take the syringe containing the sample injection portion of the water Bottles, syringe reweigh quality, and record the difference between them is the quality of the added chlorine propanol, diluted with water to the mark and mix. The solution About liquid chlorine propanol 12.5µg/mL. The solution was needed now with the current.

A.5.4.2 Sample Preparation Weigh 10g sample to the nearest 0.001g, placed in a pressure bottle was added 25 mL of sulfuric acid solution, grip the top of the bottle, and the sample rotation Move until it is fully dispersed. The bottle was placed in a boiling water bath for 10min, then swirled the bottle so that the contents were thoroughly mixed and in a boiling water bath the heating was continued for 15min, cooled to room temperature in air, and then neutralized with sodium hydroxide solution to pH = 7, dried over anhydrous sodium sulfate was added 7g and stirred with a magnetic stirrer 5min ~ 10min, until the sodium was completely dissolved, and then filtered using absorbent cotton, washed with a small amount of water pressure bottle.

The solution was transferred to a 500mL Teflon with the dispenser, respectively 50mL anhydrous diethyl ether and extracted five times, each time at least Paul extraction Hold 5min to phase separation. The ether extracts were all transferred to a graduated flask in a water bath, placed in 50 °C ~ 55 °C, the concentrated to 4mL.

NOTE. ether extract samples may contain residual impurities resolve external interference chromatogram. These residual impurities may be produced during hydrolysis degradation caused Thereof. This raises the question can be used to solve the following purification treatments. The ether extract was concentrated to approximately 8 mL in place of the above-mentioned 4 mL. Heated at 130 °C 16 h 10 g of silica and filled with a corresponding dimension of the column and gently tapping at the top of the column and 1 g of anhydrous sodium sulfate was added with 25 mL of anhydrous ether Run After the column was wet with a small amount of aid, ether extract quantitative concentrated by column. Respectively 25 mL of anhydrous ether eluted three times, collected eluate was transferred to a concentrator Concentrated to 4 mL.

The extract was cooled to room temperature, transfer with a small amount of anhydrous ether qualifier to 5.0 mL volumetric flask, diluted to the desired anhydrous ether Volume and mixed well.

A.5.4.3 Preparation of the solution still 5 pressure bottle were charged 10 g waxy maize starch, accurate to 0.001 g, 25 mL flask sulfuric acid solution. Then added 0.0 mL, 0.1 mL, 0.2 mL, 0.4 mL, 1.0 mL chloropropanols standard solution so that the concentration of starch count was 0 mg/kg, 0.1 mg/kg, 0.2 mg/kg, 0.4 mg/kg and 1.0 mg/kg. The exact calculation of the concentration of chlorine bottle propanol according to the quality standard solution chloropropanols.

Clamping bottle top, so that the sample vial swirled until completely dispersed. Then from A.5.4.2 "The bottle was placed in a boiling water bath" to get started.

A.5.4.4 Determination 1.0µL solution for injection still, each injection should have sufficient time to ensure that the appropriate signal between the peak recorded chloropropanols two isomers Completely and wash the column. Referring to the respective control samples and record the signal and the peak area plus two Chloropropanol isomers. Using the same procedure Conditions for injection concentrate extract 1.0µL samples and record the signal and the peak area plus the sample.

In each of the signal peak area still used chloropropanols isomer actual mass conversion to give chloropropanols concentration (mg/kg) plotting school N curve using the sample corresponding to the 1-chloro-2-propanol and 2-chloro-1-propanol peak area of the sample and determine the concentration of mixed chloropropanols (Mg/kg). In mastering the entire operation, and to ensure that the calibration curve from the reference sample obtained is linear and reproducible reference sample the number can be reduced to one, and mixtures containing about 5 mg/kg chloropropanols isomers.

A.5.4.5 Calculation Results Chloropropanol w1 in mg/kg according to formula (A.2) Calculated.

Where.

c-- solution for still Chloropropanol (sum of isomers) concentration in milligrams per kilogram (mg/kg);

Total area of the peak signal sample solution A1-- Chloropropanol isomer produced;

A2-- solution for still Chloropropanol isomer signal generated by the sum of the peak area.