[Determination of residues of cyromazine and its metabolite melamine in chickens by gas chromatography-mass spectrometry].
A gas chromatography-mass spectrometric (GC-MS) method has been established for the determination of cyromazine and its metabolite melamine in chickens. The homogenized tissue samples added with melamine-15N3 were extracted with acidic acetonitrile-water solution, and defatted with dichloromethane. The samples were derivatized with N,O-bis(trimethylsilyl) trifluoroacetamide (BSTFA), after solid-phase extraction (SPE) which was performed on Oasis MCX cartridges, and then detected by GC-MS. Cyromazine was quantified by an external standard method, and melamine by an internal standard method using melamine-15N3. The results indicated that the linearities of cyromazine and melamine were within the range of 100 - 1,000 microg/L, and their limits of quantification (LOQ) were 20 microg/kg. The mean recoveries of chicken samples fortified at three concentrations of 20, 40 and 80 microg/kg were within the range of 75% - 110%. The relative standard deviations (RSDs) of intra- and inter- batch were less than 10% and 15%, respectively. The application of this method was further demonstrated by analyzing 10 real samples which were brought from local markets. The results show that this method is simple, rapid, sensitive and specific. It is appropriate for the identification and quantification of cyromazine and its metabolite melamine in chickens.
Zhu
Xinle
X
China Institute of Veterinary Drug Control, Beijing, China. zhuxinle@ivdc.gov.cn
Liu
Qi
Q
Li
Dan
D
Wang
Shuhuai
S
Wang
Xia
X
D000818:Animals; D002645:Chickens; D005506:Food Contamination / Q000032:analysis; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D008460:Meat / Q000032:analysis*; D010573:Pesticide Residues / Q000032:analysis*; D014227:Triazines / Q000032:analysis*
D010573:Pesticide Residues; D014227:Triazines; C028704:cyromazine; C011907:melamine