同位素内标法测定动物源性食品中喹乙醇含量  

Isotope internal standard method for testing olaquindox in animal derived food

作　　者：张翠芬[1] 

机构地区：[1]大连职业技术学院,大连116035

出　　处：《中国食品添加剂》2017年第4期178-183,共6页China Food Additives

摘　　要：研究建立了动物源性食品中喹乙醇的高效液相色谱-串联质谱仪的残留检测方法,动物源性基质前处理采用乙腈∶乙酸乙酯(1∶1)微波超声提取两遍后浓缩,用正己烷净化,再经ZORBAXSB-C18液相色谱柱分离,0.1%甲酸水+乙腈梯度洗脱,采用高效液相色谱-串联质谱仪(带有ESI源正模式)MRM检测模式,内标法测定。方法检出限为0.5μg/kg,在0.5μg/kg^50μg/kg范围内线性相关系数r为0.9984,相对标准偏差RSD为1.9%~6.6%,回收率为93%~98%。实验前处理过程简单易行,提取率高,净化效果好,检出限低,线性相关性良好,具有较好重复性和较高回收率,定性定量准确。There sidue of olaquindox detection method in animal derived food was established byhigh performance liquid chromatography-tandem mass spectrometer for.Animal derived foodmatrix was pretreated by acetonitrile：ethyl acetate（1 ∶ 1）and extractedtwice bymicrowave ultrasonic,then purified by N-hexane.ZORBAX SB-C18 HPLC column was used in separating at gradient elutedof 0.1% Formic acid water＋acetonitrile.The final product was detected by HPLC-MS/MS（ESI＋）MRM mode.The internal standard method was used in the detection.Detectionlimit of the method is 0.5 ug/kg,at0.5μg/kg-50μg/kg range.The linear correlation coefficient r is 0.9984,repeatability RSD is1.9% ~ 6.6%,recovery is 93% ~ 98%.The pre-treatmentis simple,the extraction has high efficiency and good purification.The method has low detection limit,good linear correlation,high repeatability and recovery,and is accurate in qualitative and quantitative detection.

关 键 词：内标法 微波超声 喹乙醇 高效液相色谱-串联质谱仪 

分 类 号：TS207.3[轻工技术与工程—食品科学] TS207.5[轻工技术与工程—食品科学与工程]