GB/T 36858-2018Determination of aflatoxin B1 in feeds—High performance liquid chromatography (English PDF)

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009.

1 Scope

This standard specifies high performance liquid chromatography for the determination of aflatoxin B1 in feed.

This standard applies to the determination of aflatoxin B1 in feed ingredients, compound feed, concentrated feed, and concentrate supplements.

The detection limit of the method is 0.5 µg/kg, and the limit of quantification is 2.0 µg/kg.

2 Normative references

The following documents are indispensable for the application of this document. For dated references, only dated versions apply to this document. For undated references, the latest edition (including all amendments) applies to this document.

GB/T 6682 Analytical laboratory water specifications and test methods

GB/T 14699.1 Feed sampling

GB/T 20195 Preparation of animal feed samples

3 Principle

The aflatoxin B1 in the sample is extracted by the aflatoxin B1 extraction solution, then extracted by chloroform and derivatized with trifluoroacetic acid.

The aflatoxin B1 after birth was measured by reversed-phase high performance liquid chromatography-fluorescence detector and quantified by external standard method.

4 Reagents or materials

Only reagents identified as analytically pure were used in the analysis unless otherwise specified.

4.1 Water. It meets the primary water requirements specified in GB/T 6682.

4.2 Methanol. chromatographic grade.

4.3 Acetonitrile. chromatographic grade.

4.4 Trichloromethane.

4.5 Aflatoxin B1 extraction solution. Measure 84 mL of acetonitrile, add to 16 mL of water, and mix.

4.6 Aflatoxin B1 Derivatization Solution. Measure 20mL of trifluoroacetic acid separately, add 70mL of water, mix and add 10mL of ice B Acid, mix well. Available now.

4.7 Mobile phase. Take 20 mL of methanol, 10 mL of acetonitrile and 70 mL of water, respectively, and mix. After filtering through a 0.22 µm organic filter, it was used.

4.8 Aflatoxin B1 standard stock solution (1000µg/mL). accurately weigh aflatoxin B1 reference substance (purity >=98%) 10.0mg, Completely dissolved in 10 mL of acetonitrile to prepare a standard stock solution with aflatoxin B1 content of 1000 µg/mL, stored at -20 ° C, effective The period is 6 months. Or certified standard solution.