Wu Yingxuan, Xie Minling, Yao Yangxun, Lan Cao
Guangdong Inspection and Quarantine Technology Center, Key Laboratory of Animals and Plants and Food Import and Export of Technical Measures in Guangdong Province, Guangzhou 510623, China.
Se Pu. 2018 Aug 8;36(8):752-757. doi: 10.3724/SP.J.1123.2018.03014.
A method for the rapid and simultaneous determination of monepantel and its metabolite residues in cow and sheep milk has been developed using high performance liquid chromatography-tandem mass spectrometry. The samples were extracted with acetonitrile to precipitate the proteins and passed through a neutral alumina solid phase extraction (SPE) cartridge. The extracts were separated on an Inertsil C8-3 column (150 mm×4.6 mm, 5 μm) with a gradient elution program consisting of methanol and ammonium acetate. A triple stage quadrupole mass spectrometer equipped with an electrospray ionization source in negative ion mode was used to detect monepantel and its metabolite residues. The quantification of the analytes was performed by the external standard method. Good linear relationships between the peak areas and mass concentrations of the analytes were obtained in the range of 0.1-5.0 μg/L with correlation coefficients greater than 0.99 (=6). The limits of quantification were 2.0 μg/kg. The recoveries of the analytes in cow and sheep milk at three spiked levels (2.0, 50, and 100 μg/kg) were in the range of 90.1%-103.3% with relative standard deviations between 2.0% and 6.2% (=6). This method is fast, accurate, and highly sensitive, exhibits strong anti-interference capability with good recovery and repeatability, and can thus be used to simultaneously determine monepantel and its metabolite residues in cow and sheep milk.
建立了一种利用高效液相色谱-串联质谱法快速同时测定牛奶和羊奶中莫能菌素及其代谢物残留量的方法。样品用乙腈萃取以沉淀蛋白质,然后通过中性氧化铝固相萃取(SPE)柱。萃取物在Inertsil C8-3柱(150 mm×4.6 mm,5μm)上进行分离,采用由甲醇和醋酸铵组成的梯度洗脱程序。使用配备电喷雾电离源且处于负离子模式的三级四极杆质谱仪检测莫能菌素及其代谢物残留量。分析物的定量采用外标法。在0.1-5.0μg/L范围内,分析物的峰面积与质量浓度之间具有良好的线性关系,相关系数大于0.99(n=6)。定量限为2.0μg/kg。牛奶和羊奶中分析物在三个加标水平(2.0、50和100μg/kg)下的回收率在90.1%-103.3%范围内,相对标准偏差在2.0%-6.2%之间(n=6)。该方法快速、准确、灵敏度高,抗干扰能力强,回收率和重复性良好,可用于同时测定牛奶和羊奶中莫能菌素及其代谢物残留量。