Validation of a confirmatory method for the determination of melamine in egg by gas chromatography-mass spectrometry and ultra-performance liquid chromatography-tandem mass spectrometry.
A sensitive and reliable method was developed and validated for detection and confirmation of melamine in egg based on gas chromatography-mass spectrometry (GC-MS) and ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Trichloroacetic acid solution was used for sample extraction and precipitation of proteins. The aqueous extracts were subjected to solid-phase extraction by mixed-mode reversed-phase/strong cation-exchange cartridges. Using ultra-performance liquid chromatography and electrospray ionization in the positive ion mode, melamine was determined by LC-MS/MS, which was completed in 5 min for each injection. For the GC-MS analysis, extracted melamine was derivatized with N,O-bis(trimethylsilyl)trifluoracetamide prior to selected ion monitoring detection in electron impact mode. The average recovery of melamine from fortified samples ranged from 85.2% to 103.2%, with coefficients of variation lower than 12%. The limit of detection obtained by GC-MS and UPLC-MS/MS was 10 and 5 microg kg(-1), respectively. This validated method was successfully applied to the determination of melamine in real samples from market.
Department of Pharmacology and Toxicology, College of Veterinary Medicine, China Agricultural University, Beijing 100193, China.
Xi
X
Xia
Shuangyang
S
Ding
Xiaowei
X
Li
Xiao
X
Gong
Suxia
S
Zhang
Haiyang
H
Jiang
Jiancheng
J
Li
Jianzhong
J
Shen
D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004531:Eggs / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D052616:Solid Phase Extraction; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014227:Triazines / Q000032:analysis*; D014238:Trichloroacetic Acid / Q000737:chemistry
D014227:Triazines; D014238:Trichloroacetic Acid; C011907:melamine