超高效液相色谱-四极杆/静电场轨道阱高分辨率质谱法测定鸡肉中8种喹噁啉类药物及其代谢产物

Determination of 8 kinds of quinoxalines and their metabolites in chicken meat by applying high performance liquid chromatography-quadrupole/lectrostatic field orbit trap high resolution mass spectrometry

目的建立超高效液相色谱串联四极杆/静电场轨道离子阱高分辨率质谱法同步测定鸡肉中8种喹噁啉类药物及其代谢物的分析方法。方法鸡肉样品分别经过1%甲酸乙腈提取5种喹噁啉类原药和1 mol/L盐酸溶液提取3种代谢物,超声、振荡处理及高速离心后,分别用多重基质吸附填料和Oasis HLB固相萃取柱净化并收集,氮气吹干,用0.1%甲酸-乙腈溶液定容后合并进行分析。采用Acquity UPLC BEH C18(2.1mm×100 mm,1.7μm)色谱柱进行分离,以0.1%甲酸水和0.1%甲酸甲醇作为流动相,进行梯度洗脱。质谱采用平行反应监测模式下进行定性与定量分析。结果8种化合物能够得到较好地分离,在线性范围内线性关系良好,相关系数均大于0.999。在1、10、100 ng/g加标水平下,8种化合物平均回收率为76.1%~112.8%,相对标准偏差小于15%。方法检出限和定量限分别为0.04~0.1μg/kg和0.12~0.3μg/kg。结论本方法样品处理过程简便、分析时间短,准确可靠、灵敏度高,可用于鸡肉产品中多种喹噁啉药物的监测。

Objective To establish an analytical method for the simultaneous determination of eight quinoxalines and their metabolites in chicken by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry.Methods The chicken samples were respectively subjected to extraction of five quinoxalines prodrugs with 1%formic acid-acetonitrile and extraction of three metabolites with 1 mol/L hydrochloric acid solution.After ultrasonic treatment,oscillation treatment and high-speed centrifugation,the samples were purified and collected using multiple matrix adsorption fillers and an Oasis HLB solid-phase extraction column,respectively.The samples were blown dry with nitrogen,and fixed in volume with 0.1%formic acid-acetonitrile solution.The samples were combined for analysis.The separation was performed on an Acquity UPLC BEH C18(2.1 mm×100 mm,1.7μm)column with gradient elution using 0.1%formic acid in water and 0.1%formic acid in methanol as the mobile phase.Qualitative and quantitative analysis was performed in parallel reaction monitoring mode on the mass spectrum.Results The eight compounds could be separated well,and the linear relationship was good in the linear range,and the correlation coefficients were all greater than 0.999.At the 1,10,and 100 ng/g spiked levels,the average recoveries of the eight compounds were 76.1%-112.8%,and the relative standard deviation was less than 15%.The detection limit and quantitation limit of the method were 0.04-0.1μg/kg and 0.12-0.3μg/kg,respectively.Conclusion The method has the advantages of simple sample processing process,short analysis time,accuracy,reliability and high sensitivity,and can be used for monitoring a plurality of quinoxaline drugs in chicken products.