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
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摘要: 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(Target SIM-dd MS2)检测。所得30种染料的检出限在0.001 0~0.051 mg·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。Abstract: 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 MS2) 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.