CAJ | 학술논문

建立了一种混合型固相萃取柱净化-气相色谱-质谱法(GC-MS)测定婴幼儿配方奶粉中三聚氰酸的方法.在84 ℃条件下,用0.5%乙酸水溶液提取样品中的三聚氰酸,离心,滤液经Carb/C18混合型固相萃取柱净化,氮气吹干,硅烷化衍生,GC-MS测定,选择离子监测模式,外标法定量.在0.01～2 mg/L 内线性关系良好(r＞0.99),在0.25～2.5 mg/kg 的添加水平范围内,平均回收率为80% ～103% ,相对标准偏差(RSD)为7.7% ～14.5% ,三聚氰酸的检出限(LOD)为0.10 mg/kg,定量限(LOQ)为0.25 mg/kg.该方法快速、灵敏、准确、专一、耐用,适合婴幼儿配方奶粉中三聚氰酸的确证和定量测定.
건립료일충혼합형고상췌취주정화-기상색보-질보법(GC-MS)측정영유인배방내분중삼취청산적방법.재84 ℃조건하,용0.5%을산수용액제취양품중적삼취청산,리심,려액경Carb/C18혼합형고상췌취주정화,담기취간,규완화연생,GC-MS측정,선택리자감측모식,외표법정량.재0.01～2 mg/L 내선성관계량호(r＞0.99),재0.25～2.5 mg/kg 적첨가수평범위내,평균회수솔위80% ～103% ,상대표준편차(RSD)위7.7% ～14.5% ,삼취청산적검출한(LOD)위0.10 mg/kg,정량한(LOQ)위0.25 mg/kg.해방법쾌속、령민、준학、전일、내용,괄합영유인배방내분중삼취청산적학증화정량측정.
A method is presented for the quantitative determination and confirmation of cyanuric acid in infant formula by mixed-mode solid-phase extraction cartridge clean up-gas chromatography-mass spectrometry (GC-MS).Cyanuric acid was extracted from infant formula with an acetic acid solution at 84 ℃.An aliquot of the supernatant was cleaned up using mixed-mode solid-phase extraction cartridge containing C18 and graphitized carbon black (GCB),and evaporated to dryness under nitrogen.The residues were converted to trimethylsilyl derivatives,then determined by GC-MS in selected ion monitoring (SIM) mode.The linear range was from 0.01-2 mg/L.The recoveries were 80% -103% and the relative standard deviations were 7.7% -14.5% in the spiked range of 0.25-2.5 mg/kg.The limit of detection was 0.10 mg/kg and the limit of quantification was 0.25 mg/kg.The method is rapid,sensitive,accurate,specific,and rugged.It is suitable for the quantitative determination and confirmation of cyanuric acid in infant formula.