T/GDBK 006-2023 Determination of γ-aminobutyric acid-glyoxal-formaldehyde adduct in baked goods by high performance liquid chromatography/mass spectrometry

Scope

Scope: This document describes the principles, reagents and materials, instrumentation, sample preparation, experimental procedures, data processing, precision, and experimental reports of the high-performance liquid chromatography/mass spectrometry determination method for γ-aminobutyric acid-glyoxal-formaldehyde adducts in food. This document is applicable to the qualitative and quantitative determination of γ-aminobutyric acid-glyoxal-formaldehyde adducts in baked products. The determination of the content of products containing γ-aminobutyric acid-glyoxal-formaldehyde adducts can be referenced for use. The detection limit is 4.2 μg/kg, and the quantification limit is 13.9 μg/kg. Main technical content: 4. Principle: After degreasing the sample with n-hexane, it is extracted with a 20% methanol/water solution. The extract is evaporated under reduced pressure and re-dissolved. The sample solution is determined by the multiple reaction monitoring (MRM) mode of the high-performance liquid chromatography/mass spectrometry instrument, and quantified by the external standard method. 5. Reagents and materials 5.1 Reagents: Unless otherwise specified, all reagents are analytical grade, and the water is Grade I water as specified in GB/T 6682. Methanol (chromatography grade). N-hexane (analytical grade). Formic acid (chromatography grade). Formaldehyde (analytical grade). Glyoxal (analyzed pure). γ-Aminobutyric acid (analyzed pure). 5.2 Preparation of reagents - Methanol/water solution (20%): Transfer 50 mL of methanol (5.1.1) to a 250 mL volumetric flask and make up to the mark with water. - Formic acid/water solution (0.1%): Transfer 0.25 mL of formic acid (5.1.3) to a 250 mL volumetric flask and make up to the mark with water. 5.3 Standard sample - Standard sample of γ-aminobutyric acid-glyoxal-formaldehyde adducts (C11H16N2O4, CAS No.: 805228-41-5): Purity greater than 98.0%. 5.4 Preparation of standard solutions According to needs, prepare a solution of γ-aminobut

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