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Citation: ZHAO Shan-Zhen, YI Xiong-Hai, Cheng Jia, PAN Xiao-Bo, GUO De-Hua, ZHU Jian, DENG Xiao-Jun. Determination of 19 Kinds of Nonprotein Nitrogen Compounds in Powdered Formulas by Dispersive Solid Phase Extraction- High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2016, 44(8): 1227-1235. doi: 10.11895/j.issn.0253-3820.150938 shu

Determination of 19 Kinds of Nonprotein Nitrogen Compounds in Powdered Formulas by Dispersive Solid Phase Extraction- High Performance Liquid Chromatography-Tandem Mass Spectrometry

1.
Shanghai Entry-Exit Inspection & Quarantine Bureau, Shanghai 200135, China;
2.
Shanghai Ocean University, Shanghai 201306, China

Received Date: 25 November 2015
Revised Date: 14 March 2016

Figures(4)

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×2.1 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%.
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