高效液相色谱-串联质谱法同时检测辣椒制品中4种工业染料

Simultaneous Determination of Four Kinds of Industrial Dyes in Chili Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry

为了同时检测辣椒制品中碱性橙Ⅱ、碱性嫩黄O、罗丹明B和对位红,利用超声提取结合液相色谱-串联质谱法,采用XTerra C18柱分离,以甲醇和含0.1％甲酸的5 mmol/L乙酸铵溶液为流动相进行梯度洗脱.在正离子模式下采用多反应监测（MRM）方式进行检测,采用基质曲线外标法进行定量.辣椒制品用乙腈-水超声提取,离心后取上清液进样分析.结果表明,碱性嫩黄O、罗丹明B的线性范围均为0.2～10 μg/L,碱性橙Ⅱ、对位红的线性范围均为2～100 μg/L,且线性相关系数均大于0.99.4种工业染料的检出限为0.03～0.60 μg/kg,回收率为90.1％～116.0％,相对标准偏差为5.6％～14.8％.该方法选择性强,灵敏度高,且样品处理操作简单,适合于食品中4种非法添加工业染料的同时测定及确证分析.

An accurate method was developed for simultaneous determination of chrysoidine,auramine O,rhodamine B and para red in chili products by liquid chromatography-tandem mass spectrometry combined with ultrasonic extraction.The target analytes were separated on a Xterra C18 column with gradient elution using methanol and 5 mmol/L ammonium acetate solution containing 0.1% formic acid as mobile phase,and then detected using LC-MS/MS in multiple reaction monitoring（MRM） mode.Acetonitrile and water were used to extract the residues from chili products,and the supernatant was analyzed by chromatogram after centrifugated.The linear range of auramine O,rhodamine B was 0.2-10 μg/L,and which of chrysoidine,para red was 2-100 μg/L,the linear correlation coefficients were all more than 0.99.The LODs of four dyes were 0.03-0.60 μg/kg,the average recoveries of adding standard at six levels were 90.1%-116.0%,and the relative standard deviation of the method was 5.6%-14.8%.The method is simple,sensitive and accurate,and suitable for determination and confirmation of four industrial dyes added in chili products illegally.