• 关键词：阿维菌素检测  超快速液相色谱-串联质谱  固相萃取  制药废水

• 基金项目："十一五"国家水体污染控制与治理科技重大专项(No.2008ZX07529-006)

• 李再兴
• 1. 清华大学环境学院,北京 100084;
  2. 河北科技大学环境科学与工程学院,石家庄 050018

• 左剑恶
• 清华大学环境学院,北京 100084

• 吴春旭
• 清华大学环境学院,北京 100084

• 张敬轩
• 国家环保产品质量监督检验中心,石家庄 050015

• 李挥
• 国家环保产品质量监督检验中心,石家庄 050015

• 剧盼盼
• 河北科技大学环境科学与工程学院,石家庄 050018

• 余忻
• 清华大学环境学院,北京 100084

• 摘要：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Agilent Plus C₁₈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0.05 μg · L^-1,目标物在0.1~20 μg · L^-1范围内线性关系良好,可决系数R²=0.997.在0.1、0.5和4.0 μg · L^-1 3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.

• Abstract：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 multiple 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.

• Key words：avermectin determination  rapid resolution liquid chromatography-tandem mass spectrometry (RRLC-MS/MS)  solid phase extraction (SPE)  pharmaceutical wastewater

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