猪可食性组织中氟尼辛残留量的UPLC-MS/MS检测方法的建立

[目的] 建立一种可靠、快速、灵敏的超高效液相色谱-串联质谱法（UPLC-MS/MS）用于猪可食性组织中氟尼辛残留量的检测。[方法] 猪可食性组织（肌肉、皮脂、肝脏、肾脏）经绞碎、均质后，用乙酸乙酯-乙腈（体积比1：1）提取，MCX固相萃取柱净化，Acquity UPLC BEH C18色谱柱梯度洗脱，在电喷雾正离子（ESI+）下选用多反应监测（MRM）模式进行待测物的分析，外标法定量。[结果] 该方法的检测限（LOD）与定量限（LOQ）分别为0.5 μg？kg-1和1.0 μg？kg-1；待测物氟尼辛含量在0.5~500 μg？kg-1范围内，峰面积与药含量呈良好的线性关系（R2>0.999）；氟尼辛在猪肌肉、皮脂、肝脏、肾脏组织中的添加回收率为74.8%~90.3%，批内精密度及批间精密度均不大于16.5%。[结论] 建立了猪超高效液相色谱-串联质谱检测方法，适用于猪可食性组织中氟尼辛残留量的测定。
[Objectives] To establish a reliable, rapid and sensitive method for determination of flunixin residues in swine tissues (muscle, skin+fat, liver, kidney), ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)was developed and optimized.[Methods] The samples were extracted with acetonitrile and ethyl acetate (volume ratio 1:1), and then purified via an Oasis MCX solid-phase extraction cartridge. Chromatographic separation was performed on an Acquity UPLC BEH C18 column. The analysis was carried out on UPLC-ESI-MS/MS working with multiple reaction monitoring mode. External standard was used for quantitation of target drug.[Results] The analyte has a good linearity at the range of 0.5-500 μg？kg-1, with related coefficient of R2>0.999. Recoveries of spiked samples ranged from 74.8% to 90.3% with relative standard deviation (RSD)less than 16.5%. The limits of detection (LOD)and quantification (LOQ)were 0.5 and 1.0 μg？kg-1, respectively.[Conclusions] The results show that the pretreatment and purification process established by this study are easy to operate. The method has good stability, reproducibility, sensitivity, and great accuracy