液相色谱-串联质谱法测定土壤、沉积物和水中3种新型除草剂残留  

Determination of three new herbicide residues in soil,sediment and water by liquid chromatography-tandem mass spectrometry

作　　者：何红梅[1] 徐玲英[1] 张昌朋[1] 方楠 蒋金花[1] 王祥云[1] 俞建忠[1] 赵学平[1] HE Hongmei;XU Lingying;ZHANG Changpeng;FANG Nan;JIANG Jinhua;WANG Xiangyun;YU Jianzhong;ZHAO Xueping(State Key Laboratory for Managing Biotic and Chemical Threats to the Quality and Safety of Agro-products,Key Laboratory for Pesticide Residue Detection of Ministry of Agriculture and Rural Affairs,Institute of Agro-product Safety and Nutrition,Zhejiang Academy of Agricultural Sciences,Hangzhou 310021,China)

机构地区：[1]省部共建农产品质量安全危害因子与风险防控国家重点实验室,农业农村部农药残留检测重点实验室,浙江省农业科学院农产品质量安全与营养研究所,浙江杭州310021

出　　处：《色谱》2024年第3期256-263,共8页Chinese Journal of Chromatography

基　　金：浙江省分析测试基金项目(2018C37013)。

摘　　要：除草剂在杂草和有害植物防控上发挥着重要的作用,但其有效利用率低,大量除草剂进入环境中,对生态环境和人类健康构成了潜在威胁,因此建立环境样品中除草剂的残留分析方法尤为重要。该文采用电喷雾正离子源模式,建立了液相色谱-串联质谱法(LC-MS/MS)测定土壤、沉积物和水中异噁唑草酮、吡唑草胺和苯嘧磺草胺残留量的方法。土壤和沉积物样品经乙腈振荡提取、盐析后经C18固相萃取小柱净化,水样过滤后经C_(18)固相萃取小柱净化;再用LC-MS/MS测定样品中异噁唑草酮、吡唑草胺和苯嘧磺草胺的残留量。实验优化了仪器检测和前处理条件,考察了方法的线性关系、基质效应、检出限和定量限,并选取4种土壤、2种沉积物和水样进行了方法验证。在0.0005~0.02 mg/L范围内,异噁唑草酮、吡唑草胺、苯嘧磺草胺的线性关系均良好,r≥0.9961。3种除草剂在土壤、沉积物和水中的基质效应为-10.1%~16.5%。异噁唑草酮、吡唑草胺和苯嘧磺草胺的检出限分别为0.05、0.02、0.01μg/kg,定量限分别为0.2、0.05、0.05μg/kg。异噁唑草酮、吡唑草胺和苯嘧磺草胺在土壤、沉积物和水样中3个水平(0.005、0.1、2.0 mg/kg)下的加标回收率分别为77.2%~101.9%、77.9%~105.1%、80.8%~107.1%;相对标准偏差(RSD)分别为1.4%~12.8%、1.2%~7.7%、1.5%~11.5%。结果表明:本方法操作简单,方法稳定,定量准确,实用性强,可用于土壤、沉积物和水中异噁唑草酮、吡唑草胺和苯嘧磺草胺残留量的检测。Herbicides play an important role in preventing and controlling weeds and harmful plants and are increasingly used in agriculture,forestry,landscaping,and other fields.However,the effective utilization rate of herbicides is only 20%-30%,and most herbicides enter the atmosphere,soil,sediment,and water environments through drift,leaching,and runoff after field application.Herbicide residues in the environment pose potential risks to ecological safety and human health.Therefore,establishing analytical methods to determine herbicide residues in environmental samples is of great importance.In this study,an analytical method based on liquid chromatography-tandem mass spectrometry(LC-MS/MS)in positive electrospray ionization mode(ESI+)was developed for the determination of isoxaflutole,metazachlor,and saflufenacil residues in soil,sediment,and water.The instrumental detection parameters,including electrospray ionization mode,mobile phase,and chromatographic column,were optimized.The mobile phases were methanol(A)and 0.1%formic acid aqueous solution(B).Gradient elution was performed as follows:0-1.0 min,60%A;1.0-2.0 min,60%A-90%A;2.0-3.0 min,90%A;3.0-4.0 min,90%A-60%A;4.0-5.0 min,60%A.The samples were salted after extraction with acetonitrile and cleaned using a C_(18)solid-phase extraction column.Different solid-phase extraction columns and leaching conditions were investigated during sample pretreatment.Working curves in the neat solvent and matrix were constructed by plotting the measured peak areas as a function of the concentrations of the analytes in the neat solvent and matrix.Good linearities were found for isoxaflutole,metazachlor,and saflufenacil in the solvent and matrix-matched standards in the range of 0.0005-0.02 mg/L,with r≥0.9961.The matrix effects of the three herbicides in soil,sediment,and water ranged from-10.1%to 16.5%.The limits of detection(LODs,S/N=3)for isoxaflutole,metazachlor,and saflufenacil were 0.05,0.01,and 0.02μg/kg,respectively.The limits of quantification(LOQs,S/N=10)for isoxaflutole,

关 键 词：固相萃取 液相色谱-串联质谱 除草剂 土壤 沉积物 水 

分 类 号：O658[理学—分析化学]