建立了超高效液相色谱-四极杆飞行时间质谱（ UPLC-Q-TOF MS）快速检测水产品中15种碱性合成色素的方法。水产样品经乙腈（含10％（ v／v）乙酸）提取，采用 C18复合硅胶基质分散管进行样品净化处理。目标物采用C18色谱柱分离，以乙腈和0.1％（ v／v）甲酸-5 mmol／L 乙酸铵溶液为流动相，梯度洗脱，四极杆飞行时间串联质谱电喷雾正离子模式检测。结果表明：15种碱性色素的定量限（ LOQs，S／N=10）为0.1~100μg／kg，并在各自的线性范围内线性关系良好，相关系数（ r）≥0.993。在3个加标水平下的平均回收率为80.60％~107.37％，测定结果的相对标准偏差为3.33％~6.69％（ n=6）。该方法快速、简便、灵敏度高，适用于日常水产品中15种碱性合成色素的快速筛查。
A new method was established for the simultaneous determination of 15 basic artifi-cial dyes in fishery products by ultra performance liquid chromatography coupled with quadru-pole-time of flight mass spectrometry ( UPLC-Q-TOF MS ). The analytes in fishery products were extracted with acetonitrile containing 10%( v/v)acetic acid,then purified by dispersive solid phase extraction with C 18-silicone adsorbent. The compounds were separated by a C 18 col-umn with acetonitrile and 0. 1%( v/v)formic acid-5 mmol/L ammonium acetate solution as the mobile phases, and measured by UPLC-Q-TOF MS with electrospray ionization in positive mode. As a result,the limits of quantification( LOQs,S/N=10)of the 15 target compounds were 0. 1-100 μg/kg in fishery products. The 15 analytes behaved linearly in their respective ranges with the correlation coefficients no less than 0. 993. The average recoveries of the 15 analytes spiked at three levels were ranged from 80. 60% to 107. 37% with the RSDs of 3. 33%-6. 69%( n=6). This method is suitable for routine qualitative and quantitative analyses of the 15 basic artificial dyes in fishery products due to its fastness,simplicity and relatively high sensi-tivity.
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