液相色谱-串联质谱法快速测定食品中4种黄色工业染料

为了快速、高效的检测食品中非法添加的工业染料，为食品安全监督检测提供技术依据，建立了高效液相色谱-串联质谱法(HPLC-MS/MS)定性定量分析食品中非法添加的碱性橙Ⅱ、碱性嫩黄O、酸性橙Ⅱ、酸性金黄4种黄色工业染料。样品用乙腈提取、离心后上清液过0.22 μm聚四氟乙烯膜，电喷雾离子源多反应监测（MRM）模式检测，空白基质曲线外标法定量，其中碱性橙Ⅱ、碱性嫩黄O采用正离子扫描模式(ESI+)，酸性橙Ⅱ、酸性金黄采用负离子扫描模式(ESI-)进行检测，以超纯水(正离子扫描时水中含有0.1%甲酸)-乙腈为流动相，梯度洗脱，洗脱液流速0.3 mL/min。在优化的实验条件下，得到了较宽的线性范围和较低的定量检出限：碱性橙Ⅱ和碱性嫩黄O的线性范围均为5.0~200.0μg/L，酸性橙Ⅱ和酸性金黄的线性范围均为5.0~100.0 μg/L，线性相关系数均在0.999以上；食品中碱性橙Ⅱ、碱性嫩黄O、酸性橙Ⅱ、酸性金黄的定量限分别为50、50、75、60 μg/kg。方法的回收率和重现性较好，4种染料的回收率在75.6%~119.0%之间，相对标准偏差(RSD)在3.1%~9.1%之间。该方法操作简单、灵敏度高、结果准确可靠，可应用于食品中4种非法添加工业染料的定量及确证分析。

Rapid Determination of Four High Yellow Dyes in Foods by HPLC-MS/MS

A method based on highperformance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS)was developed for rapid determination of the residues of four yellow industrialdyes(basic orangeⅡ,auramine O, orange acidⅡandmetal yellow) in foods. The sample were extracted by acetonitrile, and thenanalyzed in multiple reaction monitoring (MRM) mode. Sample matrix-matchedcalibration was used to determine the residue contents by external standard.Basic orangeⅡand auramine O were detected with positive ion model, while orange acidⅡ, metal yellow were detected with negative ion model.The mobile phase was ultrapure water (containing 0.1% formic acid for positiveion model)-acetonitrile. Under the optimized detection conditions, the linearranges for basic orangeⅡand auramine O are 5.0-200.0μg/L, and for orange acidⅡand metal yellow are 5.0-100.0 μg/L,the linear correlation coefficients are all more than 0.999. The limits ofquantification of basic orangeⅡ,auramine O, orange acidⅡandmetal yellow are 50, 50, 75, 60 μg/kg, respectively. The recoveries of 4 dyes rangefrom 75.6% to 119.0% with relative standard deviations (RSD) of 3.1%-9.1%.This method is simple, effective, sensitive， which is suitable for the determination andconfirmation of four industrial dyes added in the foods illegally.