目的 建立液相色谱-串联质谱(LC-MS/MS)法同时测定红花中非法染色物新品红、金胺O和苏丹红Ⅳ的含量。方法 采用安捷伦EC-C₁₈(2.1 mm ×50 mm,1.8 μm)色谱柱,流动相为20 mmol/L甲酸铵+0.1%甲酸(A)和乙腈(B),梯度洗脱,流速为0.2 ml/min,柱温为 40 ℃,离子化方式为ESI,检测模式为MRM,选择离子对:(1)新品红m/z 330.3→223.2,m/z 330.3→300.2;(2)金胺O m/z 268.2→147.2,m/z 268.2→252.2;(3)苏丹红Ⅳ m/z 381.2→224.1,m/z 381.2→91.1。结果 该方法新品红、金胺O和苏丹红Ⅳ的线性范围分别为0.1086～271.50 ng/ml、0.1392～348.00 ng/ml和0.1352～338.00 ng/ml,回收率(n=6)分别为97.45%、96.44%和97.58%,RSD分别为0.70%、1.12%和0.89%,精密度、稳定性和重复性的RSD均小于3%。结论 该方法提取简单,测定方法定量准确,灵敏度高,适用于红花中非法染色物新品红、金胺O和苏丹红Ⅳ的含量测定。

Objective To develop an LC-MS/MS method for simultaneous determination of illegal dyes of New fuchsin, Auramine O and Sudan Ⅳin Carthami Flos.Methods Using Agilent EC-C₁₈(2.1 mm×50 mm,1.8 μm)column, the mobile phase consisted of 20 mmol/L ammonium formate+0.1% methane acid-acetonitrile using gradient elution. The column temperature was 40 ℃, ionization mode was ESI, and detection mode was MRM. The ion pair selected was: ①New fuchsin m/z 330.3→223.2,m/z 330.3→300.2; ②Auramine O m/z 268.2→147.2,m/z 268.2→252.2; ③Sudan Ⅳ m/z 381.2→224.1,m/z 381.2→91.1.Results The linear range of New fuchsin, Auramine O and Sudan Ⅳ was 0.1086-271.50 ng/ml, 0.1392-348.00 ng/ml and 0.1352-338.00 ng/ml, respectively, the recoveries were 97.45%, 96.44% and 97.58%, respectively, and RSD was 0.70%,1.12% and 0.89%, respectively. RSD of precision, stability and repeatability was less than 3%.Conclusions This method of extraction is simple to use, accurate for determination and highly sensitive. This method can be applied to the determination of illegal dyes of New fuchsin, Auramine O and Sudan Ⅳ in Carthami Flos.