Determination of 19 Kinds of Nonprotein Nitrogen Compounds in Powdered Formulas by Dispersive Solid Phase Extraction-High Performance Liquid Chromatography-Tandem Mass Spectrometry
10.11895/j.issn.0253-3820.150938
- VernacularTitle:基质分散固相萃取-高效液相色谱-串联质谱法快速测定婴幼儿配方乳粉中19种非蛋白氮化合物
- Author:
Shanzhen ZHAO
;
Xionghai YI
;
Jia CHENG
;
Xiaobo PAN
;
Dehua GUO
;
Jian ZHU
;
Xiaojun DENG
- Publication Type:Journal Article
- Keywords:
Dispersive solid phase extraction;
Hydrophilic interaction liquid chromatography;
Tandem mass spectrometry;
Powdered formulas;
Nonprotein nitrogen compounds
- From:
Chinese Journal of Analytical Chemistry
2016;(8):1227-1235
- CountryChina
- Language:Chinese
-
Abstract:
Abstract A method based on dispersive solid phase extraction-high performance liquid chromatography-tandem mass spectrometry for determination of 19 kinds of nonprotein nitrogen compounds including melamine, cyromazine, amidinourea, aminotriazine, 3-aminotriazole, 4-aminotriazole, allantoin, cyanuric acid, dicyandiamide, thiourea, semicarbazide, L-leucine, L-isoleucine, L-arginine, L-hydroxyproline, L-theanine, ammeline, ammelide and guanidine in powdered formulas was presented. The nonprotein nitrogen compounds were degreased by chloroform and extracted by acetonitrile, with MgSO4 to remove water and C18 to clean up. The samples were separated on Merck ZIC HILIC column (150 mm í2. 1 mm, 5 μm, 20 nm) with gradient elution. The electrospray ionization was operated in the positive mode and negative mode, and monitored by the multiple reaction monitoring ( MRM) mode. Allation was quantified by external standard method and the other 18 kinds of nonprotein nitrogen compounds were quantified by internal standard method. All of the correlation coefficients (r) were higher than 0. 99. The limits of quantitation (LOQ) were 0. 05-5. 0 mg/kg, the average recoveries were between 82 . 2% and 115 . 0%, and the relative standard deviations were less than 20%.
