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超高效液相色谱串联三重四级杆质谱分析方法检测猪肉中多种药物残留

UPLC-MS/MS Method for Determination of Multiple Drug Residues in Pork

  • 摘要: 采用80%的乙腈水溶液提取样品,使用PRiME HLB固相萃取柱进一步净化,然后氮吹浓缩,用10%甲醇水溶液复溶;以0.01%甲酸水—甲醇作为流动相,进行梯度洗脱,用超高效液相色谱串联三重四级杆质谱多反应监测模式(UPLC-MS/MS)检测分析,内标法定量。结果表明:30种药物在0.5~20.0 ng/mL浓度范围内呈现良好的线性关系,相关系数R2值介于0.993997~0.999872之间;当添加量为1.0、5.0、10.0μg/kg时,猪肉中30种药物的回收率为85.9%~115.8%;30种药物的检出限为0.02~1.00μg/kg,定量限为0.06~3.00μg/kg,表明该方法操作简便、灵敏、回收率稳定,重复性和准确性较好,适用于大批量猪肉样品的检测分析。

     

    Abstract: The samples were extracted with 80% acetonitrile solution, purified with PRiME HLB solid phase extraction column, concentrated with nitrogen, and finally dissolved with 10% methanol. A gradient elution was performed using 0.01% formic acid water-methanol as a mobile phase for gradient elution. The multi-reaction monitoring (MRM) mode of UPLC-MS/MS was used for the determination, and quantification was performed by internal standard method. The results showed that the concentration of 30 compounds showed good linearity in the range of 0.5~20.0 ng/mL, with the coefficient correlation (R2) between 0.993997 to 0.999872. At the addition levels of 1.0, 5.0 and 10.0 μg/kg, the recovery ratio of 30 compounds was 85.9%~115.8% in pork. The detection limit of 30 compounds was 0.02~1.00 μg/kg, and quantification limit was 0.06~3.00 μg/kg. The test indicated that the method was simple, sensitive, accurate, stable in recovery, good accuracy and repeatability, and suitable for the detection and analysis of large quantities of pork samples.