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.
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.
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