作者：杨彬1, 吴伟1, 石俊永2
作者单位：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
关键词：QuEChERS;气相色谱串联质谱;杀菌剂;残留
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，0.22 μm滤膜过滤，上机分析。5种农药杀菌剂的质量浓度在0.04~8.0 µg/mL浓度范围内均呈良好的线性关系。检出限如下：氟硅唑：
Determination of five fungicides residues in irrigation surface water by gas chromatography mass spectrometry
YANG Bin1, WU Wei1, SHI Junyong2
1. Cangzhou Ecological Environment Monitoring Center of Hebei Province, Cangzhou 061000, China;
2. Cangzhou Yanzhao Environmental Monitoring Technology Service Co., Ltd., Cangzhou 061000, China
Abstract: 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, 0.22 μm filter membrane was used for analysis. The results showed that there was a good linear relationship in the concentration range of 0.04 ~ 8.0 µg/mL. The detection limits were as follows: flusilazole:
μg/mL, Difenoconazole:
μg/mL, fluconazole:
μg/mL, chlorpyrimidinol:
μg/mL, azoxystrobin:
μg/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.
Keywords: QuEChERS;GC-MS/MS;fungicide;residues
2021, 47(7):60-63,98 收稿日期: 2020-09-10;收到修改稿日期: 2020-11-23
基金项目:
作者简介: 杨彬(1975-),男,河北沧州市人,高级工程师,从事环境监测和科研工作
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