GB/T 23873-2009Determination of maduramicin ammonium in feeds (English PDF)

3.1 sampling step

execution by GB/T 14699.1 requirements.

3.2 Preparation of samples

execution according to the provisions GB/T 20195 of.

4.1 Principle

Extraction feed maduramicin ammonium with acetonitrile, evaporated extract was dissolved with acetonitrile, with on - after dimethylaminobenzaldehyde solution was subjected to column Yan

Health, HPLC assay.

4.2 Reagents and materials

Unless otherwise specified, use only analytical reagent.

4.2.1

Water, GB/T 6682, level.

4.2.2 Methanol

chromatographically pure.

4.2.3 acetonitrile

chromatography.

4.2.4 tetrahydrofuran

chromatography.

4.2.5 potassium dihydrogen phosphate

pure class distinctions.

4.2.6 Phosphate

pure class distinctions.

4.2.8 sulfuric acid

pure class distinctions.

4.2.9

Phosphate - potassium dihydrogen phosphate buffer solution (pH3.0). Weigh accurately 2.04g of potassium dihydrogen phosphate (4.2.5), add 900mL water dissolved,

Plus phosphate (4.2.6) several drops of pH was adjusted to 3.0 and transferred to 1000mL volumetric flask to volume with water, shake.

4.2.10 Mobile phase

phosphate - potassium dihydrogen phosphate buffer solution (4.2.9) + tetrahydrofuran (4.2.4) + methanol (4.2.2) = 100 + 40 + 860.

4.2.11 to - dimethylaminobenzaldehyde derivatized solution

Accurately weigh 16g of - dimethylaminobenzaldehyde (4.2.7) in 1000mL brown

Vial, was added 400mL of methanol (4.2.2), stirring until completely dissolved on a magnetic stirrer, the sulfuric acid was added dropwise 8mL (4.2.8), and continue stirring until homogeneous solution was cooled to room temperature, provided with 24h.

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