GB/T 18932.24-2005Method for the determination of the metabolite residues of furaltadon,nitrofurazone,nitrofurantoin and furazolidone in honey-liquid chromatography-tandem mass spectrometry method (English PDF)

Foreword

Annex A and Annex B in this Part of GB/T 18932 are informative.

1 Scope

This Part of GB/T 18932 specifies the liquid chromatography - tandem mass spectrometry determination method for the metabolite residues of 5-methylmorpholine- 3-amino-2-yl alkyl ketones in furaltadon, semicarbazide in nitrofurazone, 1-amino-2- hydantoin in nitrofurantoin and 3-amino-2-yl alkyl ketones in furazolidone in honey.

This Part applies to the determination of the residues of 5-methylmorpholine-3-amino- 2-yl alkyl ketones, semicarbazide, 1-amino-2-hydantoin and 3-amino-2-yl alkyl ketones in honey.

The detection limit of the method in this Part. 0.2µg/kg for 5-methylmorpholine-3- amino-2-yl alkyl ketones and 3-amino-2-yl alkyl ketones; 0.5µg/kg for semicarbazide and 1-amino-2-hydantoin.

2 Normative references

The provisions in following documents become the provisions of this Part through reference in this Part of GB/T 18932. For dated references, the subsequent amendments (excluding corrections) or revisions do not apply to this Part, however, parties who reach an agreement based on this Part 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 Precision of test methods - Determination of repeatability and reproducibility for a standard test method by interlaboratory tests (GB/T 6379-1986, neq ISO 5725:1981)

GB/T 6682 Water for analytical laboratory use - Specification and test methods (GB/T 6682-1992, neq ISO 3696:1987)

3 Principle

column moist.

4 Reagents and materials

4.16 0.45µm filter membrane.

4.17 5-methylmorpholine-3-amino-2-yl alkyl ketones, semicarbazide, 1-amino-2- hydantoin and 3-amino-2-yl alkyl ketones reference material. Purity >=99%.

4.18 5-methylmorpholin-3-amino-2-yl alkyl ketone, semicarbazide, 1-amino-2- hydantoin and 3-amino-2-yl alkyl ketones standard stock solution. 1.0mg/mL. WEIGH appropriate amount of the reference material of four kinds of nitrofuran metabolites (4.17); USE methanol to prepare 1.0mg/mL standard stock solution. The stock solution shall be stored in a freezer of -18°C, away from lights; the storage period is three months.

4.19 5-methylmorpholin-3-amino-2-yl alkyl ketone, semicarbazide, 1-amino-2- hydantoin and 3-amino-2-yl alkyl ketone mixed standard working solution. 1.0µg/mL.

PIPETTE appropriate amount of the standard stock solution of four kinds of nitrofuran metabolites (4.18); USE methanol to prepare 1.0µg/mL mixed standard working solution. The standard working solution shall be stored in a freezer of -18°C, away from lights; the storage period is three months; RESUME to room temperature before use.

4.20 5-methylmorpholin-3-amino-2-yl alkyl ketone, semicarbazide, 1-amino-2- hydantoin and 3-amino-2-yl alkyl ketone mixed matrix standard calibration solution.

WEIGH 7 honey blank samples (the sample weight is 4g) in 50mL brown centrifuge tubes; ADD appropriate amount of the mixed standard working solution of four kinds of nitrofuran metabolites (4.19) in 6 blank samples respectively; OPERATE synchronously in accordance with the sample operation procedures. So that the concentration of 5-methylmorpholin-3-amino-2-yl alkyl ketone and 3-amino-2-yl alkyl

5 Instruments

5.1 Liquid chromatography - tandem quadrupole mass spectrometer, equipped with electrospray ion source.

5.2 Analytical balances. 2 balances with sensitivity of 0.1mg and 0.01g respectively.

5.3 Liquid mixer.

7 Determination steps

9 Precision

The precision data in this Part are determined in accordance with the specifications of GB/T 6379. The repeatability and reproducibility values are calculated by 95% confidence.