采用在线固相萃取-超高效液相色谱-三重四级杆复合线性离子阱质谱技术建立了水中甲磺隆、噻吩磺隆、烟嘧磺隆、氯磺隆、胺苯磺隆、苄嘧磺隆、氯嘧磺隆、吡嘧磺隆、环氧嘧磺隆、醚苯磺隆、甲嘧磺隆、氟磺隆及氟嘧磺隆13种磺酰脲类除草剂的检测方法。水样经滤膜过滤后经Oasis HLB在线柱富集净化,以Kinetex C₁₈色谱柱分离,用乙腈和0.1%甲酸水溶液梯度洗脱,采用电喷雾正离子(ESI⁺)多反应监测(MRM)信息依赖采集(IDA)增强子离子(EPI)扫描方式进行检测,外标法定量,EPI谱库确证辅助定性。结果表明,该方法在2.0~50.0 ng/L范围内线性良好(r≥0.998),加标回收率为71.4%~111.2%,相对标准偏差在2.7%~10.3%(n=6),方法检出限为0.4~0.6 ng/L,基质效应为-17.9%~13.8%。利用该方法对太湖水进行检测,结果表明,除醚苯磺隆和氟嘧磺隆外,其余11种磺酰脲类除草剂均有不同程度检出。

The method for detection of thirteen kinds of sulfonylurea herbicides,including metsulfuron-methyl,thifensulfuron-methyl,nicosulfuron,chlorsulfuron,ethametsulfuron-methyl,bensulfuron-methyl,chlorimuron-ethyl,pyrazosulfuron-ethyl,oxasulfuron,triasulfuron,sulfometsulfuron-methyl,prosulfuron and primissulfuron-methyl,in water is established by using on-line solid phase extraction (SPE)-ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with linear ion trap technology.Water samples are firstly filtrated by filter membrane,enriched and purified by HLB cartridge,then separated by Kinetex C₁₈ chromatographic column,and eluted in gradient with acetonitrile and 0.1% formic acid aqueous solution,respectively.The water samples are detected by HPLC-MS/MS in electrospray ionization source for multiple reaction monitoring of positive ions-information dependent acquisition-enhanced product ion (ESI+-MRM-IDA-EPI) mode,and the EPI library and external standard method are employed for the rapid confirmation and quantitative determination.Experimental results show that this method has a good linearity in the range of 2.0 ng·L^-1 to 50.0 ng·L^-1(r≥0.998).The recoveries are in the range of 71.4%-111.2%.The relative standard deviations range from 2.7% to 10.3% (n=6).The limit of determination is between 0.4 ng·L^-1 and 0.6 ng·L^-1.Matrix effect is -17.9% to 13.8%.As this method is used to detect the water in Taihu Lake,the other 11 sulfonylurea herbicides can be detected with the exception of etherbensulfuron and fluorosulfuron.

虞霖(1993-),男,本科,助理工程师,研究方向为水资源监测,384768448@qq.com