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«PECTINS Prepared at the 71st JECFA (2009) and published in FAO JECFA Monographs 7 (2009), superseding specifications prepared at the 68th JECFA ...»

PECTINS

Prepared at the 71st JECFA (2009) and published in FAO JECFA

Monographs 7 (2009), superseding specifications prepared at the

68th JECFA (2007) and published in FAO JECFA Monographs 4

(2007). A group ADI “not specified” was established for pectins and

amidated pectins, singly or in combination at the 25th JECFA in 1981.

INS No. 440

SYNONYMS

Consists mainly of the partial methyl esters of polygalacturonic acid

DEFINITION

and their sodium, potassium, calcium and ammonium salts; obtained by extraction in an aqueous medium of appropriate edible plant material, usually citrus fruits or apples; no organic precipitants shall be used other than methanol, ethanol and isopropanol; in some types a portion of the methyl esters may have been converted to primary amides by treatment with ammonia under alkaline conditions. Sulfur dioxide may be added as a preservative.

The commercial product is normally diluted with sugars for standardization purposes. In addition to sugars, pectins may be mixed with suitable food-grade buffer salts required for pH control and desirable setting characteristics. The article of commerce may be further specified as to pH value, gel strength, viscosity, degree of esterification, and setting characteristics.

C.A.S. number 9000-69-5 White, yellowish, light greyish or light brownish powder

DESCRIPTION

FUNCTIONAL USES Gelling agent, thickener, stabilizer, emulsifier

CHARACTERISTICS

IDENTIFICATION

Test for pectins Passes test See description under TESTS Test for amide group Passes test (amidated pectins only) Add 2 ml of concentrated hydrochloric acid and 50 ml of 60% ethanol to 0.5 g of the sample, and stir well for 20 min. Transfer to a fritted glass filter tube wash with six 10 ml portions of the HCl-60% ethanol mixture. Dissolve in 100 ml distilled water; it may be necessary to add a few drops 0.1 mol/L sodium hydroxide to achieve solution.

Transfer 4 ml of this solution into a test tube (recommended dimensions 15.5 mm inner diameter and 146 mm length). Add 1 ml 5 mol/L sodium hydroxide and mix. The mixture will form a gel. Fill a small glass tube (recommended dimensions 7.8 mm inner diameter

–  –  –

Galacturonic acid and Weigh 5 g of the sample to the nearest 0.1 mg, and transfer to a Degree of amidation suitable beaker. Stir for 10 min with a mixture of 5 ml of hydrochloric acid TS, and 100 ml of 60% ethanol. Transfer to a fritted-glass filter tube (30 to 60 ml capacity) and wash with six 15-ml portions of the HCl-60% ethanol mixture, followed by 60% ethanol until the filtrate is free of chlorides. Finally wash with 20 ml of ethanol, dry for 2.5 h in an oven at 105°, cool and weigh. Transfer exactly one-tenth of the total net weight of the dried sample (representing 0.5 g of the original unwashed sample) to a 250-ml conical flask and moisten the sample with 2 ml of ethanol TS. Add 100 ml of recently boiled and cooled distilled water, stopper and swirl occasionally until a complete solution is formed. Add 5 drops of phenolphthalein TS, titrate with 0.1 mol/l sodium hydroxide and record the results as the initial titre (V1).

Add exactly 20 ml of 0.5 mol/l sodium hydroxide TS, stopper, shake vigorously and let stand for 15 min. Add exactly 20 ml of 0.5 mol/l hydrochloric acid and shake until the pink colour disappears. Titrate with 0.1 mol/l sodium hydroxide to a faint pink colour which persists after vigorous shaking; record this value as the saponification titre (V2).

Quantitatively transfer the contents of the conical flask into a 500-ml distillation flask fitted with a Kjeldahl trap and a water-cooled condenser, the delivery tube of which extends well beneath the surface of a mixture of 150 ml of carbon dioxide-free water and 20.0 ml of 0.1 mol/L hydrochloric acid in a receiving flask. To the distillation flask add 20 ml of a 1-in-10 sodium hydroxide solution, seal the connections, and then begin heating carefully to avoid excessive foaming. Continue heating until 80-120 ml of distillate has been collected. Add a few drops of methyl red TS to the receiving flask, and titrate the excess acid with 0.1 mol/l sodium hydroxide recording the volume required, in ml, as S. Perform a blank determination on 20.0 ml of 0.1 mol/l hydrochloric acid, and record the volume required, in ml, as B. The amide titre is (B - S).

Transfer exactly one-tenth of total net weight of the dried sample (representing 0.5 g of the original unwashed sample) and wet with about 2 ml ethanol in a 50-ml beaker. Dissolve the pectin in 30 ml of

0.1 mol/l sodium hydroxide. Let the solution stand for 1 h with agitation at room temperature. Transfer quantitatively the saponified pectin solution to a 50-ml measuring flask and dilute to the mark with distilled water. Transfer 25 ml of the diluted pectin solution to a distillation apparatus and add 20 ml of Clark's solution, which consists of 100 g of magnesium sulfate heptahydrate and 0.8 ml of concentrated sulphuric acid and distilled water to a total of 180 ml.

This apparatus consists of a steam generator connected to a roundbottom flask to which a condenser is attached. Both steam generator and round-bottom flask are equipped with heating mantles.

Start the distillation by heating the round-bottom flask containing the sample. Collect the first 15 ml of distillate separately in a measuring cylinder. Then start the steam supply and continue distillation until 150 ml of distillate have been collected in a 200-ml beaker. Add quantitatively the first 15 ml distillate and titrate with 0.05 mol/l sodium hydroxide to pH 8.5 and record volume required, in ml, as A.

–  –  –

Calibration solution: Pipette 2.0 ml of standard stock solution and

2.0 ml of internal standard solution into a 200-ml volumetric flask and make up to the mark with water. Accurately weigh about 1 g of this solution (Mstandard) is filled into a head space vial and used for GC analysis.

Procedure Continue the analysis as described in Vol.4 ‘Residual solvents’, using the given conditions except for the sample heating temperature, which should be 70°, and syringe temperature, which should be 80°.

Calculation Calculate the concentration of each residual solvent using the

following equation:

–  –  –





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