气相色谱质谱法检测灌溉地表水中5种杀菌剂残留  

Determination of five fungicides residues in irrigation surface water by gas chromatography mass spectrometry

作　　者：杨彬 吴伟 石俊永 YANG Bin;WU Wei;SHI Junyong(Cangzhou Ecological Environment Monitoring Center of Hebei Province,Cangzhou 061000,China;Cangzhou Yanzhao Environmental Monitoring Technology Service Co.,Ltd.,Cangzhou 061000,China)

机构地区：[1]河北省沧州生态环境监测中心,河北沧州061000 [2]沧州燕赵环境监测技术服务有限公司,河北沧州061000

出　　处：《中国测试》2021年第7期60-63,98,共5页China Measurement & Test

摘　　要：建立测定灌溉地表用水中5种防治白粉病杀菌剂残留(氟硅唑、苯醚甲环唑、氟菌唑、氯苯嘧啶醇和嘧菌酯)的QuEChERS-气相色谱质谱的分析方法。取预处理后的水样100 mL,浓缩至近干,用30 mL 1%的冰醋酸-乙腈溶液(V∶V=1∶1)转移至50 mL离心管中;在离心管中加入2.0 g乙酸钠、5.0 g硫酸镁进行提取,涡旋3 min后,冷冻离心5 min,取出;离心后的上清液全部转移至25 mL净化管中,涡旋2 min后,冷冻离心5 min;离心后的净化液转移至刻度试管中,氮吹至近干,加丙酮1.0 mL溶解残渣,涡旋1 min后,0.22μm滤膜过滤,上机分析。5种农药杀菌剂的质量浓度在0.04~8.0µg/mL浓度范围内均呈良好的线性关系。检出限如下:氟硅唑:0.0013μg/mL、苯醚甲环唑:0.0024μg/mL、氟菌唑:0.0010μg/mL、氯苯嘧啶醇:0.0015μg/mL、嘧菌酯:0.0014μg/mL。5种农药的平均回收率在3个浓度添加水平下为87.4%~105.3%;精密度测试的相对标准偏差在1.57%~4.15%(n=6)。该方法简便快捷、效率高、准确度好,为灌溉用水中多种农药残留的监测提供一种新的分析方法。A QuEChERS GC-MS method was developed for the determination of five fungicides residues(flusilazole,Difenoconazole,fluconazole,chlorpyrimidinol and azoxystrobin)in irrigation surface water.Take 100 mL of pretreated water sample,concentrate it to nearly dry,transfer 30 mL 1%glacial acetic acid acetonitrile solution(V∶V=1∶1)into a 50 mL centrifuge tube;add 2.0 g sodium acetate and 5.0 g magnesium sulfate into the centrifugal tube for extraction,vortex for 3 min,freeze centrifugation for 5 min,and take out the supernatant;transfer all centrifuged supernatant into a 25 mL purification tube,vortex for 2 min,then freeze centrifugation for 5 min After centrifugation,the purified solution was transferred to the calibration tube,the nitrogen was blown to nearly dry,1.0 mL acetone was added to dissolve the residue,after 1 min of vortex,0.22μm filter membrane was used for analysis.The results showed that there was a good linear relationship in the concentration range of 0.04~8.0µg/mL.The detection limits were as follows:flusilazole:0.0013μg/mL,Difenoconazole:0.0024μg/mL,fluconazole:0.0010μg/mL,chlorpyrimidinol:0.0015μg/mL,azoxystrobin:0.0014μg/mL.The average recoveries of the five pesticides were 87.4%-105.3%at three concentration levels,and the relative standard deviation of precision test was in the range of 1.57%-4.15%(n=6).The method is simple,rapid,efficient and accurate.It provides a new analytical method for the monitoring of pesticide residues in irrigation water.

关 键 词：QUECHERS 气相色谱串联质谱 杀菌剂 残留 

分 类 号：X830.2[环境科学与工程—环境工程] TB9[一般工业技术—计量学]