超快速液相色谱-离子阱飞行时间质谱法测定肉制品中10种碱性染料

建立了肉制品中10种碱性染料的超快速液相色谱-离子阱飞行时间质谱(LC-IT-TOF-MS)检测方法。使用Waters AcquityTM UPLC BEH C18(100 mm×2.1 mm,1.7 μm)作为分析柱,以5 mmol/L乙酸铵水溶液-含0.1%(体积分数)甲酸的乙腈溶液为流动相进行梯度洗脱,流速0.2 mL/min。采用电喷雾离子化源,在正离子模式下进行检测。样品用乙腈提取,经弱阳离子交换(Oasis WCX)固相萃取柱净化,超快速液相色谱分离,外标法定量。结果表明,10种碱性染料在1.0～100.0 μg/L范围内线性关系良好,r2均大于0.9915,相对标准偏差(n=7)均小于8.54%。在2,10,25 μg/kg 3个添加水平下平均回收率为65.39%～119.18%。该方法简单、灵敏度高、分析时间短,适用于肉制品中多种碱性染料的同时测定。

Determination of ten basic dyes in meat products by ultra fast liquid chromatography-ion trap time of flight mass spectrometry

A method was developed for the simultaneous determination of 10 basic dyes in meat products using ultra fast liquid chromatography-ion trap time of flight mass spectrometry (LC-IT-TOF-MS). The target analytes were separated at a flow rate of 0.2 mL/min on a Waters AcquityTM UPLC BEH C18 (100 mm×2.1 mm, 1.7 μm) column with a gradient elution. The mobile phase was 5 mmol/L ammonium acetate-acetonitrile (containing 0.1%(v/v) formic acid). The identification and quantification were achieved in positive ion mode with electro spray ionization source. The samples were extracted with a simple procedure using acetonitrile and cleaned up by weak cation exchange (Oasis WCX)solid phase extraction column. Ten basic dyes were determined by LC-IT-TOF-MS, and quantified by external standard method. The developed method showed a good linearity over the wide range of 1.0~100.0 μg/L, and the relative standard deviations (n=7) were less than 8.54%. The average recoveries of the ten basic dyes at three levels (2, 10 and 25 μg/kg) were ranged from 65.39% to 119.18%. Therefore, this method, owing to its simplicity, rapidity and high sensitivity, has a good applicability to the simultaneous determination of dye residues in meat products.