UHPLC-MS/MS同位素内标法测定豆制品中16种喹诺酮类药物残留

Determination of 16 Kinds of Quinolones Residues in Soybean Products by UHPLC-MS/MS Isotopic Internal Standard Method

建立了同时测定豆制品中16种喹诺酮类药物(依诺沙星、氟罗沙星、诺氟沙星、氧氟沙星、培氟沙星、环丙沙星、洛美沙星、达氟沙星、恩诺沙星、奥比沙星、沙拉沙星、双氟沙星、司帕沙星、恶喹酸、萘啶酸、氟甲喹)残留的同位素内标结合超高效液相色谱-串联质谱法检测方法。样品用0.1 mol/L EDTA-Mcllvaine缓冲溶液提取,经HLB固相小柱净化,氮吹定容后,采用超高压反相C18色谱柱分离,质谱分析采用电喷雾电离,正离子扫描,多反应监测模式,内标法定量。在优化条件下,16种喹诺酮类药物在0.50~50.00 ng/mL的质量浓度范围内线性良好,相关系数R^2均在0.99以上,检出限(LOD)为0.5μg/kg,在检出限的1倍、2倍和10倍添加浓度下,16种喹诺酮类药物平均回收率在80.7%~107.1%之间,相对标准偏差(RSD,n=6)在1.5%~10.6%之间。该方法前处理简便快速,选择性好,灵敏度、回收率和精密度高,适用于豆制品中喹诺酮类药物残留的定性定量检测。

A method is developed for the simultaneous determination of the residues of 16 quinolones(enoxacin,fleroxacin,norfloxacin,ofloxacin,pefloxacin,ciprofloxacin,lomefloxacin,danofloxacin,enrofloxacin,orbifloxacin,sarafloxacin,difloxacin,sparfloxacin,oxolinic acid,nalidixic acid,flumequine)in soybean products by internal isotopic standard method and ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS).The sample is extracted with 0.1 mol/L EDTA-Mcllvaine buffer solution,purified by HLB solid-phase column,nitrogen volume is determined,and then separated by ultra-high pressure reverse-phase C 18 chromatographic column.Electrospray ionization,positive ion scanning,multi-reaction monitoring mode and internal standard method are used for mass spectrometry analysis.Under the optimized conditions,16 quinolones have good linearity in the mass concentration range of 0.50~50.00 ng/mL,and the correlation coefficients R^2 are all above 0.99,the detection limit(LOD)is 0.5μg/kg.Under the adding content of 1,2,10 times'detection limit,the average recovery rate of 16 quinolones ranges from 80.7%to 107.1%,and the relative standard deviation(RSD,n=6)ranges from 1.5%to 10.6%.This method is simple,rapid,with good selectivity and high sensitivity,recovery rate and precision,and it is suitable for the qualitative and quantitative detection of quinolones residues in soybean products.