超高效液相色谱测定肉制品中的罗丹明B、孔雀石绿和结晶紫及其代谢物残留

Simultaneous development of rhodamine B,malachite green,crystal violet and their metabolites residues in meat by UPLC

提出了一种以超高效液相色谱同时检测肉制品中5种违禁合成色素的新方法.以甲醇-水(V(甲醇)∶V(水)=95∶5)作为提取剂,样品在80℃经微波辅助萃取5min,继以C18固相萃取柱净化,使用ACQUITY BEH C18分析柱,以乙腈-20mmol/L乙酸铵缓冲溶液(V(乙腈)∶V(乙酸铵)=80∶20,pH=5)作流动相,实现了5种色素的有效分离.在0.1～5.0μg/mL内,校准曲线呈良好的线性,相关系数r为0.994 5～0.999 5.该方法测定肉制品中罗丹明B、孔雀石绿、结晶紫、隐性孔雀石绿和隐性结晶紫的定量限分别为4.23,1.83,1.61,1.96,1.95μg/kg.对加标50μg/kg的牛肉香肠日内测定6次,5种分析物的精密度(以RSD表示)优于9.2%.在25μg/kg和75μg/kg添加水平,平均回收率为78.01%～109.2%,相对标准偏差小于10%.实验结果表明:该方法具有快速、灵敏和准确等优点,可用于肉制品中5种违禁色素的常规分析.

A new ultra-high performance liquid chromatographic method was developed for analysis of five banned rhodamine B, malachite green, crystal violet and their metabolites residues in meat. The meat samples were extracted by microwave-assisted extraction with methanol-water （95 ： 5,V/V）, followed by clean up with C18 solid phase extraction column. The effective separation of five colorants in meat matri- xes was achieved using ACQUITY BEH C18 analytical column with acetonitrile-20 mmol/L acetic ammoni- um buffer （80 ： 20,V/V,pH=5） and no interfering peaks could be detected at the retention time of the an- alytes. The calibration curves in the range of 0.1 - 5.0 μg/mL for each analyte showed good linearity with correlation coefficients of 0. 994 5 - 0. 999 5. The method limits of quantification for rhodamme B, matachite green, crystal violet, leucomalachite green, and leucocrystal violet in meat samples were 4.23, 1.83, 1.61, 1.96, 1.95 9g/kg. For beef sausage spiked with 50 μg/kg for each analyte, the intra-day precision （as RSD） for five analytes was less than 9.2% for six determinations within a day. The average recovery of the five analytes from meat samples spiked with 25 and 75 9g/kg was 78.01%- 109.2 % with RSD% 10%. This method has the advantages of being rapid, sensitivity, and accuracy, and can be applied for multiresidue analysis of five banned and Rhodamine B food colorant in meat samples.