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同位素内标法测定动物源性食品中喹乙醇含量 被引量:2

Isotope internal standard method for testing olaquindox in animal derived food
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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.
作者 张翠芬
出处 《中国食品添加剂》 北大核心 2017年第4期178-183,共6页 China Food Additives
关键词 内标法 微波超声 喹乙醇 高效液相色谱-串联质谱仪 Internal standard method microwave ultrasonicolaquindox HPLC-MS/MS
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