UPLC-MS/MS法测野拔子蜂蜜中11种喹诺酮类药物残留  

Determination of 11 Kinds of Quinolone Residues in Honey of Elsholtzia rugulosa by UPLC-MS/MS

作　　者：田金凤[1] 尚远宏[1] TIAN Jinfeng;SHANG Yuanhong(Panzhihua University,Panzhihua 617000)

机构地区：[1]攀枝花学院,攀枝花617000

出　　处：《食品工业》2021年第4期437-440,共4页The Food Industry

基　　金：西华大学食品生物技术省高校重点实验室开放课题(szjj2017-110);攀枝花市社会发展科技计划项目(2018CY-S-28)。

摘　　要：采用超高效液相色谱串联三重四极杆质谱法测定野拔子蜂蜜中11种喹诺酮类药物残留。5.0 g样品经磷酸盐缓冲溶液(pH 3.0)提取, Oasis HLB固相萃取柱净化,采用ZORBAX SB-C18色谱柱分离,以0.2%的甲酸水溶液和40%甲醇-乙腈溶液为流动相进行梯度洗脱;质谱采用电喷雾正离子源和多反应监测模式。结果显示:11种农药在1.0~100.0μg/L浓度范围内线性关系良好,相关系数(r)>0.999,定量限为0.15~0.5μg/kg,空白样品的3个添加水平(1,5和20μg/kg)的回收率为85.9%~104.9%,δRSD为4.3%~10.5%(n=6)。该方法灵敏度及准确度良好,能满足野拔子蜂蜜中11种喹诺酮类药物残留检测的要求。This study investigated to determine 11 kinds of quinolone residues in honeyof Elsholtzia rugulosa by ultraperformance liquid chromatography-triple quadrupole mass spectrometry(UPLC-MS/MS). 5.0 g samples were extracted with phosphate buffer solution(pH 3.0), and cleaned up on the Oasis HLB cartridge. The target analytes were separated on a ZORBAX SB-C18 column with gradient elution using a mobile phase made up of 0.1% formic acid solution and 40% methanolacetonitrile solution. Positive ion of electrospray ionization(ESI) and multiple reaction monitoring(MRM) mode were adopted in MS analysis. The concentration of 11 quinolone pesticides showed good linearity in the range of 1.0-100.0 μg/L(r>0.999). The limits of detection were 0.15-0.5 μg/kg, respectively. The spiked recovery rates were in the range of 85.9%-104.9% at 3 spiked levels(1, 5 and 20 μg/kg) for blank sample, and the relative standard deviation(δRSD) was 4.3%-10.5%(n=6). The method was sensitive and accurate. It could meet the requirements for the determination of 11 kinds of quinolone residues in honey of Elsholtzia rugulosa.

关 键 词：超高效液相色谱串联三重四极杆质谱法 喹诺酮类残留 野拔子蜂蜜 

分 类 号：O657.63[理学—分析化学] S896.1[理学—化学]