Food additive - Octenyl aluminum succinate starch detection

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A. 1 Safety Reminder

Some reagents used in the inspection methods of this standard are toxic or corrosive, and caution should be exercised during operation! If splashed onto the skin, rinse immediately with water, and in severe cases, seek immediate treatment

A.2 General Provisions

Unless otherwise specified, only reagents confirmed as analytical pure and Grade III water specified in GB/T6682 shall be used in the analysis.

. The standard titration solution, impurity determination standard solution, formulation, and product used in the test method shall be prepared in accordance with the provisions of GB/T601, GB/T602, and GB/T603 unless otherwise specified; When no solvent is specified, the solution used refers to an aqueous solution

A.3 Identification Test

A.3.1 Microscopic Examination

Octenyl aluminum succinate starch that has not undergone gelatinization treatment to maintain its particle structure can be directly observed and identified by microscope to identify the shape, size, and characteristics of starch particles.

. Under the polarized light of the microscope, a typical polarized cross can be observed

A.3.2 Iodine staining

Add 1g of the sample to 20mL of water to form a suspension, and add a few drops of iodine solution. The color range should be dark blue to brownish red.

A.3.3 Copper Reduction; Preparation of alkaline copper tartrate test solution

A.3.3.1.1 Solution A: Take 34.66g of copper sulfate (CuSO4 · 5H2O), which should be free from weathering or moisture absorption, and dissolve with water to a constant volume of 500mL. Store this solution in a small sealed container

Solution B: Take 173g of potassium sodium tartrate (KNaC4H4O6 · 4H2O) and 50g of sodium hydroxide, dissolve with water to a constant volume of 500mL. Store this solution in a small alkali resistant container

Mix solution A and solution B in equal volumes to obtain alkaline copper tartrate test solution

A.3.3.2 Analysis Steps

Weigh 2.5g of the sample and place it in a flask. Add 10mL of 0.82mol/L hydrochloric acid solution and 70mL of water, mix well, reflux in a boiling water bath for 3h, and cool.

. Take 0.5mL of cooling solution and add 5mL of hot alkaline copper tartrate test solution to produce a large amount of red sediment

A.4 Determination of Octenylsuccinic Acid Group

A.4.1 Principle

After acidification and washing, the sample is titrated with alkali.

. The content of octenylsuccinic acid groups can be calculated based on the alkali consumption

A.4.2 Reagents and Materials; Isopropanol

A.4.2.2 Hydrochloric acid

A.4.2.3; Sodium hydroxide

A.4.2.4; Silver nitrate

A.4.2.5; Isopropanol solution: Measure 90mL of isopropanol, add 10mL of water, and mix well

A.4.2.6 Hydrochloric acid isopropanol solution: Take 21 mL of hydrochloric acid and place it in a 100 mL volumetric flask. Carefully dilute with isopropanol and bring to volume, shake well

A.4.2.7 Silver nitrate solution: c (AgNO3)=0.1mol/L

A.4.2.8 Sodium hydroxide standard titration solution: c (NaOH)=0.1mol/L

A.4.2.9 Phenolphthalein indicator solution: 10g/L

A.4.2.10 Starch: Undenatured starch from the same plant source

A.4.3 Instruments and Equipment

Magnetic Stirrer.

A.4.4 Analysis Steps

Weigh 5.0g of the sample to the nearest 0.001g, place it in a 150mL beaker, and wet it with a few milliliters of isopropanol.

. Add 25mL of hydrochloric acid isopropanol solution using a pipette and rinse the sample on the beaker wall with acid. Stir the sample on a magnetic stirrer for 30 minutes, add 100mL of isopropanol solution in a simple amount, and stir for another 10 minutes. Filter the sample solution using a Buchner funnel and wash the filter cake with isopropanol solution until there are no chloride ions in the filtrate (tested with silver nitrate solution). Transfer the filter cake to a 600mL beaker and wash all residual starch in the Buchner funnel with isopropanol solution into the beaker. Add water to bring the total volume to 300mL. After stirring the sample in a boiling water bath for 10 minutes, add phenolphthalein indicator solution and titrate it with sodium hydroxide standard titration solution while hot until the phenolphthalein endpoint is reached. Perform a blank test on starch (A.4.2.10)

A.4.5 Result Calculation

The mass fraction w0 of the octenylsuccinic acid group is calculated according to formula (A.1):

In the formula:

V1- The volume of sodium hydroxide solution consumed by the titration sample, in milliliters (mL)

V0- Volume of sodium hydroxide solution consumed for titration blank, in milliliters (mL)

c - concentration of sodium hydroxide solution, in moles per liter (mol/L)

M - Molar mass of octenylsuccinic anhydride, in grams per mole (g/mol) [M (C12H18O3)=21.20]

m - mass of the sample, in grams (g)

1000- Conversion factor

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