GB 25531-2010The national food safety standards of food additives sucralose (English PDF)

Foreword

Appendix A of this standard is a normative appendix.

National Food Safety Standard

Sucralose Food Additive

1 Scope

This standard applies to sugar as raw material, a chlorine atom optionally substituted three hydroxyl groups prepared food additive sucralose.

2 Normative references

The standard file referenced in the application of this standard is essential. For cited documents with dates, only the date of

Version applies to this standard. For undated references, the latest edition (including any amendments) applies to this standard.

3 chemical name, molecular formula, molecular mass and structural formula

4 Technical Requirements

1 x - xx

xx =

XMA

PMAX

US

sU (A.1)

Where.

Content X1-- sucralose sample,%;

AU-- liquid chromatography sample mean peak area;

MS-- weighed sucralose standard mass in grams (g);

P-- sucralose content standards in marked sucralose,%;

AS-- mean standard solution chromatogram peak area;

MU-- saying that the quality of the sample taken, in grams (g);

X0-- measured moisture content of the sample,%.

The results parallel arithmetic mean of the measurement results shall prevail. Twice in the same condition absolutely independent determination results

The difference is not more than 2% of the arithmetic mean.

A.4 Determination of specific rotation

A.4.1 Weigh about 1 g sample (accurate to 0.00 1g), dissolved in water, transferred to a 100 mL volumetric flask, add water to the mark, shake

uniform. The measurement temperature was 20 degrees C +/- 0.5 degrees C.

Specific rotation alpham (20 degrees C, D) value to (°) . dm2 . kg-1 according to formula (A.2) Calculated.

(A.2)

Where.

alpha - measured angle of rotation, in degrees (°);

l - the length of the optical tube unit decimeter (dm);

rhoalpha - mass concentration in the solution effective component in grams per milliliter (g/mL).

A.4.2 Other conducted in accordance with GB/T 613-2007 in.

Determination A.5 hydrolyzate

A.5.1 Reagents and materials

a) p- anisidine.

b) phthalic acid.

c) methanol.

d) mannitol.

e) fructose.

A.5.2 Instruments and Equipment

TLC plates. silica gel coated with Merk 60 or other equivalent materials 0.25mm thickness.

()

alpharho

alphaalpha

DCm = °, 20

A.5.3 Analysis step

Preparation of the toner was A.5.3.1

The 1.23g p- anisidine and 1.66 g phthalic acid dissolved in 100 mL of methanol. The solution was kept in the dark and refrigerated, if dissolved

Failure was already fading.

A.5.3.2 Preparation of standard solution A

Weigh 10g mannitol (accurate to 0.001g), dissolved in water and transferred to 100mL volumetric flask with water to volume.

A.5.3.3 Preparation of standard solution B

Weigh 10g mannitol (accurate to 0.001g) and 0.04g fructose (accurate to 0.0001g), transferred to 100mL volumetric flask

With water to volume.

A.5.3.4 Preparation of sample solution

Weigh 2.5g sample (accurate to 0.001g), was dissolved with 5mL methanol, transferred to a 10mL volumetric flask with methanol to

Scale.

A.5.4 Determination

Take standard solution A, B standard solution and the sample solution each 5µL, respectively, in different locations with a TLC plate spotting,

Each solution will be 5 times (each time 1µL) points on the board, to be spotted between each sample point and then continue drying, 3 parts of sample area

To basically the same, After spotting is finished with a chromogenic reagent spray after 100 degrees C +/- 2 degrees C oven heating 15min, immediately after heating in a dark background

Observed chromatography plate, the sample solution should not be deeper than the coloring stain stain blush standard solution B.

Note. If the spotting point standard solution A blackened, indicating chromatography plate is heated for too long, it must be remade.

A.6 Determination of related substances

A.6.1 Reagents and materials

a) Sucralose Standard. mass fraction >=98.0%.

b) acetonitrile.

c) sulfuric acid.

d) methanol.

e) NaCl. 50g/L.

A.6.2 Instruments and Equipment

TLC plate. 0.2mm thickness coated with C18 alkyl modified silica gel or other equivalent material.

A.6.3 Analysis step

A.6.3.1 Preparation Agent Expand

Developing solvent. sodium chloride solution. acetonitrile = 70.30 (ratio by volume).

Preparation of the toner was A.6.3.2

Preparation of a methanol solution of 15% sulfuric acid (volume fraction).

A.6.3.3 Preparation of standard solutions

Weigh 0.5g sucralose standard (accurate to 0.001g), was dissolved in 5.0mL of methanol, and this is the solution C. Draw 0.5mL

Solution C, with methanol to 100mL, this is the solution D.

A.6.3.4 Preparation of sample solution

Weigh 1.0g sample (accurate to 0.001g), was dissolved in 10.0mL of methanol.

A.6.4 Determination

Take the solution C, D and solution of each sample solution 5µL, point to the bottom of the TLC plate, the plate is placed chromatography developing solvent containing the chromatography tank

, The solvent front to move to be expanded after removing 15cm TLC plate placed to be the agent evaporate after use color sprays,

Then heated at 125 +/- 2 degrees C degrees C oven for 10min. Rf value of the sample solution should be the primary stain solution C Rf value the same as the main spots and the specimen

Other liquid stains should be no deeper than the coloring solution D main stain coloration.

Rf value - after the sample spots to expand distance from the origin to the solvent front and the ratio of the distance from the origin.

A.7 Determination of methanol

A.7.1 Reagents and materials

a) Methanol Standard. chromatography.

b) n-propanol. chromatography.

c) pyridine. chromatography.

A.7.2 Instruments and Equipment

Gas chromatograph. with hydrogen flame ionization detector.

A.7.3 reference chromatographic conditions

a) Column. 2.1m x 4mm (inner diameter) glass column, within 0.2mm ~ 0.15mm polystyrene chromatographic stationary phase filling; or

He is equivalent to the column.

b) Carrier gas. nitrogen or helium.

c) Column temperature. 150 degrees C.

d) Inlet temperature.200 degrees C.

e) Detector temperature. 250 degrees C.

f) flow rate. 20mL/min.

g) Injection volume. 1µL.

NOTE. System Suitability standard solution is injected twice repeated, resulting in response to the relative error is less than 2.0% area.

A.7.4 Analysis step

A.7.4.1 Preparation of internal standard solution

Imbibe 1.0mL n-propanol, placed in 100mL flask with pyridine to volume, shake. The solution was pipetted 5mL,

Placed in 500mL flask with pyridine to volume, shake.

A.7.4.2 Preparation of standard solutions

Imbibe 2.0mL methanol, placed in 100mL flask, with internal standard solution to volume, shake. Pipette 1.0mL of the solution

It was placed in 100mL flask, with internal standard solution to volume, shake.

A.7.4.3 Preparation of sample solution

Weigh about 2g sample (accurate to 0.001g), was dissolved with the internal standard solution and transferred to 10mL volumetric flask, using the internal standard solution to volume

Mark and shake.

A.7.5 Determination

In A.7.3 reference chromatographic conditions, respectively, the standard solution and the sample solution was measured injection volume was 1 µL, a repeat injection

Second, calculate the peak area ratio of methanol and the internal standard peak area of each injection.

A.7.6 Calculation Results

X2 methanol content according to formula (A.3) Calculated.

10000158.02 xx

x =

US

MR

RX% (A.3)

Where.

X2-- sample methanol content,%;

RU-- two injections of the sample solution in methanol and internal standard (n-propanol) average ratio of peak areas;

0.00158-- concentration standard solution in methanol x x bulk density of the sample solution in methanol (2 x 10-4 x 0.79 x 10);

RS-- two injections standard solution of methanol and internal standard (n-propanol) average ratio of peak areas;

MU-- saying that the quality of the sample taken, in grams (g).

The results parallel arithmetic mean of the measurement results shall prevail. Twice in the same condition absolutely independent determination results

The difference is not more than 10% of the arithmetic mean.