1 Scope
This standard specifies the LC-MS-MS method for determining the altrenogest and chlormadinone residues in fugu, eel and baked eel.
This standard is applicable to the confirmation and quantitative determination of altrenogest and chlormadinone residues in fugu, eel and baked eel.
Method detection limit of this standard: the detection limit of altrenogest and chlormadinone is 0.5μg/kg.
2 Normative references
The following normative documents contain provisions which, through reference in this text, constitute provisions of this standard. For dated references, subsequent amendments (excluding corrections), or revisions, of any of these publications do not apply to this standard, however parties to agreements based on this standard are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition applies.
GB/T 6379.1 Accuracy (trueness and precision) of measurement methods and results - Part 1: General principles and definitions (GB/T 6379.1-2004, ISO 5725-1:1994, IDT)
GB/T 6379.2 Accuracy (trueness and precision) of measurement methods and results - Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method (GB/T 6379.2-2004, ISO 5725-2:1994, IDT)
GB/T 6682 Water for analytical laboratory use - Specification and test methods (GB/T 6682-2008, ISO 3696:1987, MOD)
3 Principle
After the specimen is enzymatically hydrolyzed for 16h at 37℃, the altrenogest and chlormadinone residues in the specimen are extracted with acetonitrile, and the extracting solution is degreased with acetonitrile saturated n-hexane, purified by solid phase extraction column, and ionized with electrospray, then detected and confirmed with LC-MS-MS method, and quantified with external standard method.
Foreword i
1 Scope
2 Normative references
3 Principle
4 Reagents and materials
5 Instruments and apparatus
6 Specimen preparation and preservation
7 Determination steps
8 Result calculation
9 Precision
Annex A (Informative) Multi-reaction monitoring (MRM) chromatograms of standard solution
Annex B (Informative) Recovery rate