GB/T 22509-2008Animal and vegetable fats and oils -- Determination of benzo(a)pyrene -- Reverse-phase high performance liquid chromatography method (English PDF)

Foreword

This standard, through modification, adopts the ISO 15302.2007 Animal and

vegetable fats and oils – Determination of benzo (alpha) pyrene – Reverse-phase

high performance liquid chromatography method (English version).

As compared with ISO 15302.2007, the main technical differences are as

follows.

- DELETE the noun terminology;

- Appropriately MODIFY the instrument and equipment;

- ADD the measurement methods for the alumina activity;

- CHANGE the elution reagent petroleum ether (40 °C ~ 60 °C) or n-hexane

into petroleum ether (30 °C ~ 60 °C) or n-hexane;

- CHANGE the constant volume of the tested solution from 250 µL to 100 µL;

CHANGE the sample injection volume from 50 µL to 10 µL;

- CHANGE the internal standard method quantitative calculation into the

external standard quantitative calculation.

Annexes A, B, C and D of this standard are informative.

This standard was proposed by the State Grain Administration.

This standard shall be under the jurisdiction of the National Grain and Oil

Standardization Technical Committee.

The drafting organizations of this standard. Dalian City Product Quality

Supervision and Inspection Institute, the State Food Quality Supervision and

Inspection Center, Dalian Standard Detection Technology Research Center.

1 Scope

This standard specifies the principles, reagents and materials, apparatus and

equipment, sampling method, sample preparation, operation procedures, test

results presentation, precision and so on for the determination of benzo (a)

pyrene in animal and vegetable fats and oils through the reverse-phase high

performance liquid chromatography method.

This standard applies to animal and vegetable fats and oils.

The minimum detection limit of this standard method is 0.1 µg/kg.

The measurement range of this standard is 0.1 µg/kg ~ 50 µg/kg.

2 Normative references

The provisions in following documents become the provisions of this standard

through reference in this Standard. For the dated references, the subsequent

amendments (excluding corrections) or revisions do not apply to this standard;

however, parties who reach an agreement based on this standard are

encouraged to study if the latest versions of these documents are applicable.

For undated references, the latest edition of the referenced document applies.

GB/T 6379.2 Accuracy (trueness and precision) of measurement methods

and results - Part 2. Basic methods for the determination of repeatability and

reproducibility of a standard measurement method (GB/T 6379.2-2004, ISO

5725-2.1994, IDT);

GB/T 6682 Water for analytical laboratory use – Specification and test

methods (GB/T 6682-2008, ISO 3696.1987, MOD);

GB/T 15687 Oils and fats – Preparation of test sample (GB/T 15687-1995,

eqv ISO 661.1989)

5 Instruments and equipment

6 Sampling method

The samples received by the laboratory shall be representative, AND the

samples shall not be damaged or altered during transport and storage.

This standard does not specify the sampling method, AND it is recommended

to use the sampling method as specified in GB/T 5524.

b) Column. Polycyclic aromatic hydrocarbon analysis column, 4.6 mm × 250

mm;

c) Sample injection volume. 10 µL;

d) Mobile phase. acetonitrile . water = 880 .120 (volume ratio);

e) Flow rate. 1.0 mL/min;

f) Fluorescence detector. emission wavelength. 406 nm (slit. 10 nm),

excitation wavelength. 384 nm (slit. 10 nm).

9 Presentation of test results

The benzo (a) pyrene content is calculated using the equation (1).

Where.

Appendix A

(Informative)

Brockmann alumina activity measurement methods

A.1 Definition of activity

Depending on the water content, the neutral alumina can be divided into five

activity levels. Based on Brockmann's definitions, the level I alumina is the

alumina which is fired at 450 °C for 12 h; whilst the level II, III, IV and V

alumina is produced by respectively adding 3%, 6%, 10% and 15% of water

into the level I alumina.

A.2 Measurement

A.2.1 Chromatographic column. glass column, Phi 15 mm × H 150 mm, the

lower part is cushioned with a little absorbent cotton, FILL 50 mm height

alumina; MAKE it tight.

A.2.2 Reagents. benzene + petroleum ether (1 +4).

A.2.3 Activity test solution preparation. based on the following combinations,

respectively TAKE 20 mg of each kind of azo dye; USE the reagent (A.2.2) to

set the volume in a 50mL volumetric flask, to prepare the corresponding dye

mixed solution.

The first pair (I). azobenzene (AB) and p-methoxazobenzene (MAB);

The second pair (II). MAB and Sudan I (Sudan I, S I);

The third pair (III). Sudan...

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