QuEChERS/超高效液相色谱-串联质谱法测定大黄鱼中非法染料硫代黄素

建立了超高效液相色谱-串联质谱法测定大黄鱼中硫代黄素残留的分析方法.样品中的硫代黄素经乙腈-水溶液提取,QuEChERS方法净化,C18色谱柱分离,以0.1％(体积分数)甲酸水溶液-乙腈为流动相进行梯度洗脱,三重四极杆质谱电喷雾多反应监测模式检测,外标法定量.结果表明,硫代黄素为0.5～50.0 ng/mL时线性关系良...

Determination of illegal dyes thioflavine T in Larimichthys crocea by QuEChERS-UPLC-MS/MS

An analytical method was developed for the determination of thioflavine T in Larimichthys crocea using ultra-performance liquid chromatography-tandem mass spectrometry. The samples were extracted with an acetonitrile-water solution and purified by the quick, easy, cheap, effective, rugged and safe(QuEChERS) method. The separation was carried out on a C₁₈column with gradient elution using 0.1%(V/V) formic acid aqueous solution and acetonitrile as mobile phases by ultra-performance liquid chromatography(UPLC). The target compound was detected by MS/MS system with electrospray ionization(ESI) under multiple reaction monitoring(MRM) mode with external standard method. Under the optimal conditions, thioflavine T showed good linearity(r>0.998) in the range of 0.5-50.0 ng/mL. The limit of detection(LOD) of the method was 2.0 μg/kg and the limit of quantitation(LOQ) was 5.0 μg/kg. Moreover, the spiked recoveries of the analyte from blank Larimichthys crocea samples at the three levels of 5.0, 20.0 and 100.0 μg/kg were in the range of 94.1%-99.2% with the relative standard deviations(RSD) less than 1.60%. With the advantage of convenience, fast, sensitivity and good repeatability, the method is suitable for the detection of thioflavine T in Larimichthys crocea.