分析化学Issue(8)：1227-1235,9.DOI:10.11895/j.issn.0253-3820.150938
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
Determination of 19 Kinds of Nonprotein Nitrogen Compounds in Powdered Formulas by Dispersive Solid Phase Extraction-High Performance Liquid Chromatography-Tandem Mass Spectrometry
摘要
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%.关键词
基质分散固相萃取/亲水相互作用色谱/串联质谱法/婴幼儿配方乳粉/非蛋白氮化合物Key words
Dispersive solid phase extraction/Hydrophilic interaction liquid chromatography/Tandem mass spectrometry/Powdered formulas/Nonprotein nitrogen compounds引用本文复制引用
赵善贞,伊雄海,程甲,潘孝博,郭德华,朱坚,邓晓军..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[J].分析化学,2016,(8):1227-1235,9.基金项目
本文系上海市技术标准专项(No.15DZ0503201),长三角联合攻关项目(No.15395810100)资助 （No.15DZ0503201）
