摘要
建立了固相萃取(SPE)/超高效液相色谱-三重四极杆串联质谱(UPLC-MS/MS)同时测定水中8种苯氧羧酸类除草剂残留的方法。过滤后的样品经HLB固相萃取柱富集净化后,采用BEH C18柱,以2 mmol/L乙酸铵-乙腈作为流动相进行梯度洗脱,采用串联质谱进行检测。8种苯氧羧酸类除草剂在0.8～100μg/L质量浓度范围内线性关系良好(r=0.995 8～0.999 6),回收率为74%～90%,相对标准偏差为1.0%～12.0%,方法检出限(3S)为1.0～1.8 ng/L。该方法快速、灵敏,适用于水体中8种苯氧羧酸类除草剂残留的测定。
The analysis of pesticides in water samples is a problem of primary concern to quality control laboratories due to the toxicity level of these compounds and their public health risk. A method for the analysis of eight phenoxy acid herbicide residues in water was developed using solid phase extraction（SPE） combined with ultra performance liquid chromatography -tandem mass spectrometry （UPLC -MS/MS）. The water samples were extracted and cleaned with HLB SPE column. The extract was separated on a BEH Cl8 column using acetonitrile -2 mmol/L aqueous ammonium acetate as mobile phase with a linear gradient elution program, and analyzed by MS under negative ion mode with multiple reaction monitoring（MRM） mode. The calibration curves of eight phenoxy acid herbi- cides were linear in the concentration range of 0. 8 - 100 μg/L, with correlation coefficients of 0. 995 8 -0. 999 6. The spiked recoveries ranged from 74% to 90% , with relative standard deviations of 1.0% - 12.0%. The detection limits （3S） were between 1.0 ng/L and 1.8 μg/L. The method was simple, rapid, sensitive and accurate, and was suitable for the simultaneous determination of eight phenoxy acid herbicides in surface water and waste water.
出处
《分析测试学报》
CAS
CSCD
北大核心
2013年第1期89-93,共5页
Journal of Instrumental Analysis
基金
2009年度国家环境保护标准制修订项目(929)
江苏省2008年环境监测科研基金项目计划(0821)
