液相色谱—质谱联用法测定生猪尿中多残留物

Determination of multiple residues in swine urine by liquid chromatography-mass spectrometry

建立了生猪尿中克仑特罗、莱克多巴胺、沙丁胺醇残留检测的(HPLC-MS/MS)。猪尿经酶解后,通过调pH值9. 5、用OasisMCX萃取柱子依次用5mL甲醇,5mL水活化,取备用液全部过柱,再依次用5mL水、5mL2%的甲酸水溶液、5mL甲醇淋洗,减压抽干,用5mL 5%的氨水甲醇溶液洗脱,洗脱液在50℃下用氮气吹干,残余物用0. 5mL的甲醇水(1∶9)定容,同时对样品基质影响的分析、净化过程的质谱条件、梯度洗脱条件等进行了优化得出了较好的实验效果。

A method of determining clenbuterol, ractopamine and salbutamol residues in swine urine （HPLC -MS/MS） was established. After swine urine was enzymatic hydrolyzed, and pH value was adjusted to 9.5, and OasisMCX extraction column was activated with 5 mL methanol and 5 mL water in order, and reserve liquid all passed column, then it was leached with 5 mL water, 5 mL 2% formic acid - water and 5 mL methanol in order, and it was drained under reduced pressure. It was eluted with 5 mL 5% ammonia water methanol solution, and the eluate was evaporated to dryness at 50℃ by nitrogen, and residue was reconstituted by 0.5 mL methanol - water （ 1 ： 9 ）. Meanwhile, the effect of sample matrix was analyzed, and the mass spectrometry conditions in purification process, the gradient elution conditions and others were optimized, and better experiment result was obtained.