超快速液相色谱-串联质谱法测定制药废水中阿维菌素的研究

Determination of avermectin in pharmaceutical wastewater by rapid resolution liquid chromatography-tandem mass spectrometry

建立了采用固相萃取-超快速液相色谱-串联质谱(SPE-RRLC-MS/MS)测定制药废水中阿维菌素残留的方法.水样经离心、沉淀蛋白质后,上清液采用HLB固相萃取柱富集和净化;以0.1%甲酸水溶液和50%～90%甲醇为流动相,采用AgilentPlusC18柱进行RRLC分离,在串联质谱ESI(+)模式下采用多反应监测模式(MRM)进行检测.方法的阿维菌素检出限为0.05μg.L-1,目标物在0.1～20μg.L-1范围内线性关系良好,可决系数R2=0.997.在0.1、0.5和4.0μg.L-13种浓度添加水平下平均回收率为73.31%～111.03%,相对标准偏差为4.97%～9.37%.该方法灵敏度高、重现性好、定性定量准确,可满足制药废水中痕量阿维菌素残留检测的要求.

A method based on solid phase extraction-rapid resolution liquid chromatography-tandem mass spectrometry （SPE-RRLC-MS/MS） was developed to determine avermectin in pharmaceutical wastewater. Water samples were firstly purified through centrifugation and protein precipitation processes, and then the avermectin was enriched and purified with HLB SPE, separated through Agilent Plus C18 RRLC （rapid resolution liquid chromatography） using 0.1% formic acid solution and 50% to 90% methanol as mobile phase, and detected by mass spectrometry in positive ion mode with muhiple reaction monitoring （MRM） using an electrospray ionization interface. The detection limit was 0.5 μg.L-1. The linear range was 0. 1 μg.L-1 to 20 μg.L-1, with a coefficient of determination of 0. 997. The recoveries at spiked concentrations of 0.1 μg.L-1 , 0. 5 μg.L-1 and 4.0 μg.L-1 ranged from 73.31% to 111.03 % , with a relative standard deviation （RSD） from 4.97% to 9.37 %. The procedure provides a rapid, reliable and sensitive method for determination of avermectin in pharmaceutical wastewater.