超高效液相色谱-串联质谱法测定兔肉中喹乙醇代谢物残留量  

Determination of Olaquindox Metabolite Residues in Rabbit by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：肖利龙[1] 花锦 

机构地区：[1]太原学院,山西太原030032 [2]山西出入境检验检疫局,山西太原030024

出　　处：《农产品加工（下）》2015年第12期53-54,57,共3页Farm Products Processing

摘　　要：采用超高效液相色谱-串联质谱法,建立测定兔肉中喹乙醇代谢物3-甲基喹恶啉-2-羧酸的方法。样品经乙腈-乙酸乙酯溶液和乙腈溶液依次提取,流动相定容后采用Waters BEH C_(18)色谱柱(5μm,150 mm×2.0 mm)分离,以甲醇水溶液梯度洗脱,以串联质谱在多反应监测(MRM)正离子模式下检测,基质外标法定量。结果表明,喹乙醇质量浓度在5~200 ng/m L范围内线性良好,相关系数R^2=0.999 4。样品在3个添加水平下平均回收率为76.0%~100.5%,变异系数为1.5%~3.6%。该方法简单、灵敏、稳定,适用于兔肉中喹乙醇代谢物的检测和确证。A method has been developed for the determination of olaquindox metabolite in rabbit by ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）. The target analyte is extract from samples with acetonitrile-ethyl acetate solution and acetonitrile solution in turn. The separaction of compounds is carried on a Waters BEH C18 column（5 μm,150 mm×2.0 mm） by gradient elution using aqueous methanol solution as mobile phase. The analyte is detected by tandem mass spectrometry under multiple reaction monitoring（MRM） mode with positive electrospray ionization. And it was quantified by the matrix-matched external standard method. The results show that the calibration curve of olaquindox metabolite is linear in the range of 5200 ng/m L with correlation coefficients is 0.999 4. The average recoveries of olaquindox metabolite at spiked concentration three different levels which are oranged from 76.0% to 100.5% with relative standard deviations of 1.5%3.6%. The result show that the method is sensitive, accurate, and suitable for the determination and confirmation of olaquindox metabolite in rabbit.

关 键 词：喹乙醇 3-甲基喹恶啉-2-羧酸 超高效液相色谱-串联质谱 兔肉 

分 类 号：TS207.5[轻工技术与工程—食品科学]