Bo Haibo, Pang Guofang, Luo Lili, Cao Yanzhong
Qinghai Entry and Exit Inspection and Quarantine Bureau, Xining 810000, China.
Se Pu. 2009 Mar;27(2):149-52.
A sensitive and selective method is presented for the determination of levamisole residues in milk and milk powder by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Levamisole in the test samples was extracted with ethyl acetate under alkaline condition, then transferred into dilute hydrochloric acid, and cleaned-up with a strong cation exchange (SCX) column to obtain an extract suitable for the analysis by UPLC-MS/MS. Levamisole was separated by a BEHC18 UPLC column and acetonitrile-1.0% formic acid (15:85, v/v) as mobile phase, and electrospray ionization was applied and operated in the positive ion mode. The calibration curve was good linear between the peak area and the mass concentration of levamisole from 2.0 to 100.0 microg/L with the correlation coefficient of 0.997. The average recoveries of levamisole spiked in milk and milk powder samples at the three concentrations ranged from 64.5% to 102.0% with the relative standard deviations less than 13.1%. The detection limits of levamisole were 0.4 microg/kg in milk and 2 microg/kg in milk powder.
建立了一种灵敏且具选择性的超高效液相色谱-串联质谱法(UPLC-MS/MS)测定牛奶和奶粉中左旋咪唑残留量的方法。测试样品中的左旋咪唑在碱性条件下用乙酸乙酯萃取,然后转移至稀盐酸中,并用强阳离子交换(SCX)柱净化,以获得适合UPLC-MS/MS分析的提取物。采用BEHC18 UPLC柱,以乙腈-1.0%甲酸(15:85,v/v)为流动相分离左旋咪唑,采用电喷雾电离并在正离子模式下运行。左旋咪唑的峰面积与质量浓度在2.0至100.0μg/L之间呈良好线性,相关系数为0.997。在牛奶和奶粉样品中添加的三个浓度水平的左旋咪唑平均回收率在64.5%至102.0%之间,相对标准偏差小于13.1%。牛奶中左旋咪唑的检出限为0.4μg/kg,奶粉中为2μg/kg。