用Waters AcQuity BEH Hilic亲水色谱柱-超高效液相色谱法测定了饲料中纳多洛尔的含量。样品先后2次用1%(φ)酸化甲醇溶液15,10 mL超声提取,合并两次上清液,并分取5 mL,通过MCX SPE小柱净化。用5%(φ)氨化甲醇溶液5 mL洗脱。洗脱液在40 ℃用吹氮蒸干。残渣用由乙腈、0.5%甲酸溶液和水以体积比10比15比75组成的混合液1 mL溶解,分取1.0 μL进行色谱分析。采用亲水色谱柱为固定相及上述乙腈-甲酸溶液-水的混合液作流动相,纳多洛尔得到很好分离,纳多洛尔的质量浓度在0.01~20 mg·L-1之间与峰面积呈线性关系。方法的测定下限(10S/N)为0.01 mg·kg-1。用标准加入法测得回收率在78.5%~95.0%之间,测定值的相对标准偏差(n=5)均小于8%。

The hydrophilic chromatographic column, Waters AcQuity BEH Hilic column was used in UHPLC determination of nadolol in feed. The sample was extracted ultrasonically twice with 15, 10 mL of 1% (φ) methanol. The supernatants were combined. An aliquot of 5 mL was taken and purified by passing through MCX SPE micro-column. The column was eluted with 5 mL of mixture of 5% (φ) CH3OH and NH3 (aq.). The eluate was evaporated to dryness by N2-blowing at 40 ℃, and the residue was taken up with 1 mL of the mobile phase which is a mixture of acetonitrile, 0.5% formic acid solution, and water, mixed in the ratio of 10 to 15 to 75. An aliquot of 1.0 μL was introduced and analyzed by UHPLC. Satisfactory separation of nadolol was attained by using the Hilic column and the above mentioned mixture as mobile phase. Linear relationship between values of peak area and mass concentration of nadolol was kept in the range of 0.01-20 mg·L-1. Lower limit of determination (10S/N) found for the method was 0.01 mg·kg-1. Values of recovery found by standard addition method were ranged from 78.5% to 95.0%, with values of RSD′s (n=5) less than 8%.