QuEChERS样品前处理-高效液相色谱法测定动物组织中那西肽残留量

Determination of Nosiheptide Residues in Animal Tissues by QuEChERS Coupled with High Performance Liquid Chromatography

关键词:  那西肽  残留量  动物组织  高效液相色谱法

Key words:  nosiheptide  residues  animal tissues  HPLC

摘要:

建立了QuEChERS样品前处理-高效液相色谱法测定鸡、猪组织中那西肽残留量的方法。动物组织样品中残留的那西肽用乙腈提取，经C18和无水硫酸镁分散固相萃取净化，旋转蒸干复溶后，用高效液相色谱-荧光检测器测定。方法在0.01 ~ 2.0 μg/mL的线性范围内，线性相关系数r2为0.9998；检测限和定量限分别为5 μg/kg和10 μg/kg。在10~100 μg/kg添加浓度范围内，猪、鸡肌肉和肝脏等动物组织中那西肽平均回收率为73.8%~93.0%，批内相对标准偏差（RSD）在1.3%~11.1%之间，批间相对标准偏差（RSD）在2.9%~10.9%之间。该方法条件易于控制，结果准确，重现性好，适用于动物组织中那西肽残留量的测定。

Abstract:

A QuEChERS sample pretreatment coupled with high performance liquid chromatography (HPLC) method for the determination of nosiheptide in animal tissues was optimized and validated. The swine and poultry tissues were extracted by acetonitrile, and a QuEChERS purifing method with C18 and MgSO4 was followed. Finally,the extraction was evaporated (40 ℃) and residue was dissolved in mobile phase. A Waters Symmetry C18 colmun（250 mm×4.6mm，5μm）was employed for separation. As the results showed, the calibration graph was linear between 0.01 μg/mL to 2.0 μg/mL for nosiheptide (r2=0.9998), and the limit of detection (LOD) was 5 μg/kg, and the limit of quantitation (LOQ) was 10 μg/kg. Recoveries of nosiheptide in swine and poultry tissues were between 73.8% and 93.0%, when its additive concentrations were between 10 μg/kg and 100 μg/kg, the RSD for within-run assays were 1.3%~11.1% and RSD for between-run assays were 2.9%~10.9%. It was concluded that this method was simple, sensitive and reliable for determination of nosiheptide residues in animal tissues.