1 Scope
This standard specifies the GC-MS method for the determination of melamine, ammelide, ammelide and cyanuric acid in original plant products.
It is applicable to the determination of melamine, ammeline, ammelide and cyanuric acid in wheat flour, corn flour and rice flour.
2 Principle
The sample is extracted with a solvent, and the extracting solution is concentrated by a nitrogen blowing instrument and then derived with a silylating reagent. The melamine, ammeline, ammelide and cyanuric acid are detected and confirmed by GC-MS in the selected ion monitoring mode, and quantified by the external standard method.
3 Reagents and materials
Unless otherwise specified, all reagents used are analytical reagent and the water is distilled water or water with equivalent purity.
3.1 Diethylamine
3.2 Acetonitrile: chromatographically pure.
3.3 Pyridine: purity ≥99%.
3.4 Silylating reagent: N, O-bis (trimethylsilyl) trifluoroacetamide (BSTFA) containing 1% trimethyl chlorosilane (TMCS).
3.5 Extracting solvent: diethylamine - water - acetonitrile (10+40+50, volume ratio).
3.6 Melamine: purity ≥99.0%, CAS No.: 108-78-1.
3.7 Ammeline: purity ≥99.0%, CAS No.: 645-93-2.
3.8 Ammelide: purity ≥99.5%, CAS No.: 645-92-1.
Foreword i
1 Scope
2 Principle
3 Reagents and materials
4 Instruments and apparatus
5 Specimen preparation and preservation
6 Analytical procedures
7 Calculation of results
8 Determination lower limit
9 Recovery rate and precision
Annex A (Informative) Retention time, selection of monitoring ions and relative abundance of melamine, ammelide, ammeline and cyanuric acid
Annex B (Informative) Total ion chromatogram of derivatives of melamine, ammelide, ammeline and cyanuric acid and mass spectrum of each derivative in full scan mode
Annex C (Informative) Added recovery and precision of melamine, ammelide, ammeline and cyanuric acid in wheat flour, corn flour and rice flour
Standard
GB/T 22288-2008 Determination of melamine ammeline ammelide and cyanuric acid in original plant products - GC-MS method (English Version)
Standard No.
GB/T 22288-2008
Status
valid
Language
English
File Format
PDF
Word Count
5000 words
Price(USD)
120.0
Implemented on
2008-12-1
Delivery
via email in 1 business day
Detail of GB/T 22288-2008
Standard No.
GB/T 22288-2008
English Name
Determination of melamine ammeline ammelide and cyanuric acid in original plant products - GC-MS method
1 Scope
This standard specifies the GC-MS method for the determination of melamine, ammelide, ammelide and cyanuric acid in original plant products.
It is applicable to the determination of melamine, ammeline, ammelide and cyanuric acid in wheat flour, corn flour and rice flour.
2 Principle
The sample is extracted with a solvent, and the extracting solution is concentrated by a nitrogen blowing instrument and then derived with a silylating reagent. The melamine, ammeline, ammelide and cyanuric acid are detected and confirmed by GC-MS in the selected ion monitoring mode, and quantified by the external standard method.
3 Reagents and materials
Unless otherwise specified, all reagents used are analytical reagent and the water is distilled water or water with equivalent purity.
3.1 Diethylamine
3.2 Acetonitrile: chromatographically pure.
3.3 Pyridine: purity ≥99%.
3.4 Silylating reagent: N, O-bis (trimethylsilyl) trifluoroacetamide (BSTFA) containing 1% trimethyl chlorosilane (TMCS).
3.5 Extracting solvent: diethylamine - water - acetonitrile (10+40+50, volume ratio).
3.6 Melamine: purity ≥99.0%, CAS No.: 108-78-1.
3.7 Ammeline: purity ≥99.0%, CAS No.: 645-93-2.
3.8 Ammelide: purity ≥99.5%, CAS No.: 645-92-1.
Contents of GB/T 22288-2008
Foreword i
1 Scope
2 Principle
3 Reagents and materials
4 Instruments and apparatus
5 Specimen preparation and preservation
6 Analytical procedures
7 Calculation of results
8 Determination lower limit
9 Recovery rate and precision
Annex A (Informative) Retention time, selection of monitoring ions and relative abundance of melamine, ammelide, ammeline and cyanuric acid
Annex B (Informative) Total ion chromatogram of derivatives of melamine, ammelide, ammeline and cyanuric acid and mass spectrum of each derivative in full scan mode
Annex C (Informative) Added recovery and precision of melamine, ammelide, ammeline and cyanuric acid in wheat flour, corn flour and rice flour
