离子对-超高效液相色谱串联质谱多反应监测快速测定肉制品中的酸性橙Ⅱ、酸性橙Ⅲ、酸性橙AGT

Fast Determination of Three Acid Orange Dyes:Acid Orange Ⅱ,Acid Orange Ⅲ and Acid Orange AGT in Meat Products by Ion-pair Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了超高效液相色谱-串联质谱(UPLC-MS/MS)测定肉制品中酸性橙Ⅱ、酸性橙Ⅲ、酸性橙AGT的快速分析方法。用含5%氨水的乙腈溶液对样品进行提取,采用弱阴离子交换柱富集净化,在ESI负离子源模式下采用多反应监测(MRM)模式进行检测。通过在流动相中加入离子对试剂乙酸二己基铵(DHAA),使目标物在C18色谱柱上实现了分离,并有效改善了目标组分的离子化效率,使监测离子对更加稳定,确保了检测结果的稳定性和灵敏度。该方法分析时间小于6 min,线性范围为5.0～300μg/L,相关系数(r)大于0.999,检出限(LOD,S/N=3)为20.0～50.0μg/kg,定量下限(LOQ,S/N=10)为70.0～170.0μg/kg,方法回收率为83%～89%,精密度RSD≤7.5%。该方法快速、灵敏,适用于肉制品中3种酸性橙污染物的检测与确证。

A method based on ultra performance liquid chromatography - tandem mass spectrometry （UPLC - MS/MS） was developed for the simultaneous determination of three industrial acid dyes, namely acid orange Ⅱ, acid orangeⅢ and acid orange AGT, in meat products. The samples were extracted with acetonitrile （ containing 5% ammonia ）, cleaned up and enriched with WAX solid phase extraction（SPE） cartridge, and then analyzed by UPLC -MS/MS under the multiple reaction monitoring（MRM） mode. All the analytes were successfully detected in negative ion mode by adding an ion-pair reagent of dihexylammonium acetate（DHAA） to the mobile phase in 6 min. The calibration curves were linear between 5.0 μg/L and 300 μg/L, and the correlation coefficients（r） were more than 0. 999. The limits of detection （ LOD, S/N = 3 ） and the limits of quantitation （ LOQ, S/N= 10） were in the range of 20. 0 -50. μg/kg and 70. 0 - 170μg/kg, respectively. The spiked recoveries were in the range of 83% - 89% , and relative standard deviations （ RSD, n = 3） were no morethan 7.5%. The method was simple, effective and sensitive, and was suitable in the determination and confirmation of three industrial acid orange dyes in the meat product samples.