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.
Xia
Xi
X
Department of Pharmacology and Toxicology, College of Veterinary Medicine, China Agricultural University, Beijing 100193, China.
Ding
Shuangyang
S
Li
Xiaowei
X
Gong
Xiao
X
Zhang
Suxia
S
Jiang
Haiyang
H
Li
Jiancheng
J
Shen
Jianzhong
J
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