Key Laboratory of Chemical Biology and Traditional Chinese Medicine Research, Ministry of Education, Hunan Normal University, Changsha, P. R. China.
J Sep Sci. 2010 Sep;33(17-18):2688-97. doi: 10.1002/jssc.201000262.
A hydrophilic interaction liquid chromatography coupled to ESI-MS (HILIC/ESI-MS) method for the simultaneous determination of melamine and related compounds, i.e. ammeline, ammelide and cyanuric acid in foods was developed and validated. The separation was accomplished on a Venusil HILIC column with a mobile phase of acetonitrile + 10 mM ammonium formate buffer solution at pH 3.5 (88:12, v/v) under isocratic elution mode. For the detection of the targets, the ESI probe worked in the positive and negative switching mode. For each compound, three ions were selected as qualitative ions to obtain high specificity, and the most abundant ion of each compound was selected for quantification to obtain high sensitivity. The target compounds were quantified using SIM with 15N3-melamine and 13C3-cyanuric acid being used as an internal standards in the positive and negative modes, respectively. Compared with RP separation mode, HILIC has merits such as high separation and anti-interference efficiency. The method validation including linearity, LOD, LOQ, precision and recovery proved that the method has merits such high sensitivity, specificity and simplicity versus the other methods reported in the literature.
建立并验证了一种亲水作用色谱-电喷雾串联质谱（HILIC/ESI-MS）法，用于同时测定食品中三聚氰胺及相关化合物，即三聚氰胺亚胺、三聚氰胺酰胺和三聚氰酸。采用 Venusil HILIC 柱，以乙腈+10 mM 甲酸铵缓冲溶液（pH 3.5）（88:12，v/v）为流动相，在等度洗脱模式下进行分离。ESI 探头在正、负切换模式下用于检测目标物。对于每种化合物，选择三个离子作为定性离子，以获得高特异性，选择每种化合物中最丰富的离子进行定量，以获得高灵敏度。采用 SIM 定量，正、负模式下分别以 15N3-三聚氰胺和 13C3-三聚氰酸作为内标。与 RP 分离模式相比，HILIC 具有高分离和抗干扰效率等优点。方法验证包括线性、LOD、LOQ、精密度和回收率，结果表明，与文献报道的其他方法相比，该方法具有灵敏度高、特异性强、操作简单等优点。
