超高效液相色谱-串联质谱测定土壤中磺胺类药物残留  

Determination of Sulfonamides in Soil by Μltra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：吕燕[1] 赵健[1] 杨挺[1] 吴银良[1] 张雪艳[2] 

机构地区：[1]农业部农产品质量安全监督检验测试中心,宁波315040 [2]通标标准技术服务有限公司青岛分公司,青岛266102

出　　处：《现代仪器与医疗》2014年第2期51-57,共7页Modern Instruments & Medical Treatment

基　　金：农业部农业重大重点项目(2013C11003);宁波市农业攻关项目(2011C10005)

摘　　要：建立了固相萃取- 超高效液相色谱三重四级杆质谱联用法测定土壤中痕量的18 种磺胺类残留的方法,土样提取液经过固相萃取富集净化后由液相色谱分离、三重四级杆质谱检测.该方法在10 min 内完成对18 种目标化合物的分析.磺胺类线性范围为1 ～ 100μg/L,相关系数均大于0.995,6 次空白加标重复测定的相对标准偏差（n=6） 为1.8%～ 15.9%.l8 种目标化合物的方法检出限在0.05 ～ 0.48 μg/kg 之间,实际样品的加标回收率为64.9%～ 104%.该方法操作简便,重现性好,可用于土壤中磺胺类的检测.A rapid analytical method for determination of sixteen sulfonamides in soil was developed.Soil samples were purifi ed and concentrated by solid phase extraction(SPE)then analyzed by ultra performance liquid chromatography electrospray tandem mass spectrometry(UPLC-MS/ MS).The analysis of SAs can be finished in 10 minutes.The linear ranges were 1-100ug/L for sulfonamides,respectively.All the correlation coefi cients were more than 0.995.The relative standard deviations of spiked blank samples( =6)were 1.8%-15.9% for sulfonamides,respectively.The limits of determination for analyses were in the range of 0.05-0.48 μg/kg.The average recovery rate of real samples was in the range of 64.9%-104%.The method is simple and has good repeatability,it is suitable for determination of Sas in soil sample.

关 键 词：磺胺类 液质联用 固相萃取 

分 类 号：O657[理学—分析化学]