四种固相萃取柱在猪肉中四种氟喹诺酮类药物残留UPLC法检测中的应用比较

Application of Kinds of SPE Cartridges in the Detection of Fluoroquinolones from Pork by UPLC

中文关键词:  固相萃取  氟喹诺酮  检测  液相色谱

英文关键词:solid phase extraction(SPE)  fluoroquinolone  detection  liquid chromatography

中文摘要:

      目的 本文研究比较了四种固相萃取(solid phase extraction, SPE)柱在超高效液相色谱(ultra performance liquid chromatography, UPLC)法检测猪肉中四种氟喹诺酮类药物的应用效果。方法 首先标液过SPE柱实验, 从中筛选出回收率符合要求的三种SPE柱, 再对其进行3水平、6平行的加标试验。加标试验添加含量以环丙沙星计为20、60、200 μg/kg。结果 三种SPE柱即HLB 3 cc、Agilent C18 1 cc和Supelclean LC-C18 1 mL都有较好的净化效果, 回收率和稳定性均能满足检测要求, 其中HLB 3 cc柱的回收率为87.3%~101.2%, RSD为0.2%~5.2%; Agilent C18 1 cc柱的回收率为89.0%~100.0%, RSD为1.0%~3.6%; Supelclean LC-C18 1 mL柱的回收率为83.7%~97.2%, RSD为0.7%~6.6%。在10~100 μg/L浓度范围内线性关系良好, 相关系数R>0.999, 检出限为0.1~1.3 μg/kg, 定量限为0.1~4.2 μg/kg。结论 三种SPE柱均能用于猪肉中四种氟喹诺酮类药物残留检测。

英文摘要:

      Objective Four kinds of SPE cartridges were applied and compared in the detection of drug residues of four fluoroquinolones in pork by UPLC. Methods Standard solutions were purified by four kinds of SPE columns, in which three kinds of columns were selected for their satisfying recoveries. Then recovery experiment was developed on three levels for 20, 60, 200 μg/kg with six parallels. Results The results showed that the three SPE cartridges (HLB 3 cc, Agilent C18 1 cc and Supelclean LC-C18 1 mL) had satisfying purification effect, and recovery rate and stability could meet the requirements of detection. For HLB 3cc cartridge, the recoveries were 87.3%~101.2% and RSD were 0.2%~5.2%. For Agilent C18 1 cc, the recoveries were 89.0%~100.0% and RSD values were 1.0%~3.6%. For Supelclean LC-C18 1 mL, the recoveries were 83.7%~97.2% and RSD values were 0.7%~6.6%. The linear relation was good when the concentration range was 10~100 μg/L and the correlation coefficient was over 0.999. Limit of detection was 0.1~1.3 μg/kg and limit of quantification was 0.1~4.2 μg/kg. Conclusion Three kinds of SPE columns can be applied for detection of four fluoroquinolones residues in pork.