UPLC-MS/MS法同时测定动物油脂中11种喹诺酮类兽药残留

Simultaneous determination of 11 fluoroquinolones residues in animal oil by UPLC-MS/MS

应用固相萃取技术作为方法前处理,建立了动物油脂中11种喹诺酮类兽药残留超高效液相色谱串联质谱(UPLC-MS/MS)检测方法。样品经过正己烷溶解,80%乙腈水提取,PRIMEHLB柱净化后,经BEHC18(50mm×2.1mm,1.7μm)分离,以乙腈和0.1%甲酸+2mmol/L甲酸铵水为流动相进行梯度洗脱,11种喹诺酮在5.0min中内完成分析检测。方法的最低检测限为1.0μg/kg,在0.1~5.0ng/mL浓度范围内,11种喹诺酮类兽药线性良好,相关系数均在0.99以上;加标回收率在80%-110%,变异系数≤10%。该方法检测流程简单,净化效果好,灵敏度高,可满足实际样品分析的需求。

Solid phase extraction (SPE) was used as a pretreatment method to establish a method for the determination of 11 fluoroquinolones residues in animal oils by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).The samples were dissolved in n-hexane, extracted with 80% acetonitrile water, purified by PRIME HLB column, separated by BEH C18 (50 mm ×2.1 mm, 1.7 μm), and gradiently eluted with acetonitrile and 0.1% formic acid + 2 mmol/L ammonium formate water as mobile phase. The analysis of 11 fluoroquinolones was completed within 5.0 minutes. The minimum detection limit of the method is 1.0 μg/kg. Within the concentration range of 0.1-5.0 ng/mL, the linearity of 11 fluoroquinolones veterinary drugs is good, and the correlation coefficient is above 0.99. The recovery of standard addition is 80%-110%, and the coefficient of variation is less than 10%. The method has the advantages of simple detection process, good purification effect and high sensitivity, and can meet the needs of actual sample analysis.