QuEChERS前处理高效液相色谱-串联质谱法 同时测定食品中6种工业染料

Simultaneous determination of 6 kinds of industrial dyes in food using QuEChERS sample preparation and high performance liquid chromatography-tandem mass spectrometry

中文关键词:  QuEChERS  调味品  豆制品  肉制品  工业染料  高效液相色谱-串联质谱法

英文关键词:QuEChERS  condiment  bean products  pot-stewed meat products  industrial dyes  high performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立食品中6种工业染料的QuEChER前处理高效液相色谱-串联质谱同时测定方法。方法 均匀样品用水分散溶解后, 加乙腈提取, 经改进的QuEChERS方法净化, 0.22 μm微孔滤膜过滤, 用0.1%甲酸-5 mmol/L乙酸铵溶液和乙腈为流动相梯度洗脱, C18柱分离, 分别在电喷雾正、负离子模式下以多反应监测方式检测, 外标法定量。结果 结果表明, 6种工业染料在0.5~40 μg/L浓度范围内与其呈良好的线性关系(r＞0.999), 检出限为1.0~2.0 μg/kg, 在添加水平为1.0、5.0、20 μg/kg时, 平均回收率为76.1%~114.8%, 相对标准偏差(RSD)为2.0%~9.7%(n=6)。结论 该方法分析速度快, 灵敏可靠, 重复性好, 适用于调味品、豆制品、卤肉制品、红糖等食品中6种工业染料的测定。

英文摘要:

      Objective To develop a new method for simultaneous determination of 6 kinds of industrial dyes in food by QuChERS sample preparation and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The homogenized samples were dispersed by water, then the analyte were extracted with acetonitrile, purified by improved QuEChERS method, and filtered through 0.22 μm millipore membrane. The filtrate was detected by HPLC-MS/MS, identified by electrospray ionization (ESI) in positive and negative mode under multiple reaction monitoring (MRM) mode, and quantified with external standard method. The sample extracts were separated on a C18 column by gradient elution with acetonitrile-containing 0.1% formic acid and 5 mmol/L ammonium acetate water solution as mobile phase. Results The method showed good linear relationships in the range of 0.5~40 μg/L of 6 kinds of industrial dyes, and the correlation coefficients were more then 0.999. The limits of quantitation (LOQ) for samples were between 1.0 and 2.0 μg/kg. The average recovery rates were 76.1~114.8% at spiked levels of 1.0, 5.0, and 20 μg/kg. The relative standard deviations (RSD, n=6) were 2.0%~9.7%. Conclusion The method is fast, sensitive, reliable and reproducible for the determination of 6 kinds of industrial dyes in condiments, bean products, pot-stewed meat products, brown sugar and so on.