摘要
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.
出处
《分析测试学报》
CAS
CSCD
北大核心
2012年第10期1229-1235,共7页
Journal of Instrumental Analysis
基金
浙江省质量技术监督局科技计划项目(20100206
20090208)
浙江省分析测试研究项目(2009F70033)
关键词
超高效液相色谱串联质谱
多反应监测
酸性橙Ⅱ
酸性橙Ⅲ
酸性橙AGT
离子对
肉制品
食品安全
ultra performance liquid chromatography tandem mass spectrometry
multi reaction mo-nitoring
acid orange ]I
acid orange 11I
acid orange AGT
ion-pair
meat product
food safety