超高压液相色谱-轨道阱质谱法测定加工食品中30种禁用工业染料

Determination of 30 Forbidden Industrial Dyes in Processed Food by UHPLC-Orbitrap Mass Spectrometry

采用超高压液相色谱-四极杆静电场轨道阱质谱法测定食品中30种禁用工业染料。样品用乙腈-丙酮-氨水（66＋33＋1）混合液提取，所得提取液经Oasis HLB和中性氧化铝串联固相萃取柱净化后进行色谱分离，用Thermo Gold C18柱作固定相，并以不同体积比的乙腈和0．1％（φ）甲酸溶液的混合液作流动相进行梯度淋洗。质谱分析中，采用电喷雾正离子源和选择离子扫描-数据依赖的二级采集模式（TargetIM—dd MS^2）检测。所得30种染料的检出限在0．0010～0．051mg·kg^-1之间。加标回收率在85．2％～96．5％之间，相对标准偏差（n=6）在2．1％～9．8％之间，质量的相对偏差在±5×10^-6以内。

UHPLC-electrostatic quadrupole/orbitrap mass spectrometry was applied to the determination of 30 forbidden industrial dyes in processed food. The sample was extracted with acetonitrile-acetone-aqueous ammonia （66＋33＋ 1） mixture, and the extract obtained was purified on HLB and neutral alumina solid-phase extraction column. The purified extract was separated by HPLC using Thermo Gold C18 column as stationary phase, and mixtures of acetonitrile and 0. 1% （φ） formic acid solution in various ratios as mobile phase in gradient elution. Electrospray ionization positive ion source and the mode of Target Selected Ion Monitoring-Data Dependent MS2 scanning （Target SIM-dd MSe） were adopted in the mass spectrometry. Detection limits for the 30 forbidden industrial dyes were in the range of 0. 001 0-0. 051 mg· kg^-1. Recovery was tested by standard addition method, giving results in the range of 85.2%-96.5%, with RSDs （n=6） ranged from 2. 1% to 9. 8%. The mass relative deviation was within ±5× 10^-6