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GB 29930-2013: Food additive -- Hydroxypropyl starch
Status: Valid

Standard ID	Contents [version]	USD	STEP2	[PDF] delivered in	Standard Title (Description)	Status	PDF
GB 29930-2013	English	209	Add to Cart	3 days [Need to translate]	Food additive -- Hydroxypropyl starch	Valid	GB 29930-2013

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Basic data

Standard ID	GB 29930-2013 (GB29930-2013)
Description (Translated English)	Food additive -- Hydroxypropyl starch
Sector / Industry	National Standard
Classification of Chinese Standard	C54
Classification of International Standard	67.020
Word Count Estimation	9,943
Regulation (derived from)	China Food & Drug Administration [2013] No. 234, November, 1, 2013
Issuing agency(ies)	National Health and Family Planning Commission of the People's Republic of China
Summary	This standard applies to food additives: hydroxypropyl starch. Hydroxypropyl starch This standard is also applicable the enzymatic treatment, acid treatment, alkali treatment, bleached processed.

GB 29930-2013: Food additive -- Hydroxypropyl starch

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Food additive-Hydroxypropyl starch National Standards of People's Republic of China National Food Safety Standard Hydroxypropyl starch food additives Issued on. 2013-11-29 2014-06-01 implementation National Food Safety Standard Hydroxypropyl starch food additives

1 Scope

This standard applies to edible starch or arrowroot starch produced by a starch milk raw material obtained as a raw material to react with the etherification agent prepared Food additives hydroxypropyl starch, and a combination of enzymatic treatment, acid treatment, alkali treatment, bleaching treatment and pre-gelatinized treatment of one or more Food additive method after processing hydroxypropyl starch.

2 Technical Requirements

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 etherifying agent type and amount. propylene oxide, no more than 25% by mass of dry starch. 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 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 Pasting process without holding hydroxypropyl starch granule structure of starch granules can be directly observed identify shapes, sizes and special microscope Sign. 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 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 hydroxypropyl A.4.1 Principle Hydroxypropyl starch in sulfuric acid to generate propylene glycol, propylene glycol propionaldehyde further dehydrated alcohols and propylene, both dehydrated product sulfur Purple acid medium can generate complex with ninhydrin. 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 ℃ 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 0   fc 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, 30 m × 0.32 mm (inner diameter), filling polyethylene glycol 20M (PEG20M). A.5.3.2 oven temperature. temperature programming, 50 ℃ heat 5 min, at a rate of 10 ℃/min raised to 220 ℃, heat 2 min. A.5.3.3 Inlet temperature. 250 ℃. A.5.3.4 detector temperature. 250 ℃. 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 10 μL 5 μL syringe take chloropropanols. Weigh the syringe and quality chloropropanols injection containing 500 mL portions of water Flask, reweigh the syringe quality, and record the difference between them is the quality of the added chlorine propanol, diluted with water to the mark and mix. The chlorine-propanol solution was approximately 12.5 μg/mL. The solution was needed now with the current. A.5.4.2 Sample Preparation Weigh 10 g samples, accurate to 0.001 g, 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 10 min, then swirled the bottle its contents well mixed, and in boiling water Bath heating was continued 15 min, cooled to room temperature in air, and then neutralized with sodium hydroxide solution to pH = 7, was added 7 g anhydrous sulfur Sodium and stirred for 5 min ~ 10 min using a magnetic stirrer until the sodium was completely dissolved, then use cotton wool filtered, washed with a small amount Pressure bottle. The solution was transferred to a 500 mL Teflon with the dispenser, and separately with 50 mL of anhydrous ether and extracted five times, each time extraction Take for at least 5 min to phase separation. All ether extracts were transferred to a water bath at a graduated flask, placed in 50 ℃ ~ 55 ℃, the Concentrated to 4 mL. NOTE. ether extract samples may contain analytic extraneous residual impurities interfere with the 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 ℃ 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 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 Still inject 1.0 μL of solution, each injection should have sufficient time to ensure chloropropanols between two isomers of the corresponding signal peak record Record 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 Operating conditions inject 1.0 μL concentrated extract of the sample, and add a recording signal and the peak area of the sample. In each of the signal peak area still used chloropropanols isomer actual mass conversion to give chloropropanols concentration (mg/kg) plotting The calibration curve using the sample corresponding to 1-chloro-2-propanol and 2-chloro-1-propanol peak area and determine the concentration of the sample 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. Ac  .. (A.2) Where. c-- solution for still Chloropropanol (sum of isomers) concentration in milligrams per kilogram (mg/kg); Signal peak sum of the areas of the sample solution A1-- Chloropropanol isomer produced; A2-- solution for still Chloropropanol isomer signal generated by the sum of the peak area.