摘要
[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 C_(18)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0.5μg·kg-1和1.0μg·kg^(-1);待测物氟尼辛含量在0.5~500μg·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 coeffi- cient 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.
出处
《南京农业大学学报》
CAS
CSCD
北大核心
2017年第6期1105-1110,共6页
Journal of Nanjing Agricultural University
基金
农业行业标准制定与修订(农产品质量安全)项目(2014)