固相萃取-超高效液相色谱-三重四级杆串联质谱法测定水中4种杀菌剂

建立了固相萃取-超高效液相色谱-三重四级杆串联质谱方法检测水中4种杀菌剂(嘧菌酯、戊唑醇、吡唑醚菌酯、肟菌酯). 水样中的杀菌剂经HLB固相萃取柱富集后，使用C18色谱柱分离，以高效液相色谱-串联质谱(HPLC-MS/MS)外标法定量分析. 同时考察pH值、洗脱溶剂、洗脱量等对杀菌剂萃取效果的影响. 试验结果表明，4种化合物在0.10~50.0 μg/L浓度范围内具有较好的线性关系，检出限在0.004~0.095 μg/L之间，回收率为68.7%~95.4%，相对标准偏差(n=5)低于10%. 方法操作简单、快速、准确、灵敏度高，适用于水中4种杀菌剂的定量分析.

Detection of 4 Fungicides in Water by Solid Phase Extraction- Ultra-High Performance Liquid Chromatography-Triple Quadrupole Tandem Mass Spectrometry

A solid phase extraction-ultra-high performance liquid chromatography-triple quadrupole mass spectrometry method has been established to detect four fungicides (azoxystrobin, tebuconazole, pyrazole ether ester and oxime ester) in water. The fungicides in water samples were enriched on a HLB solid phase extraction column, separated on a C18 chromatographic column, and analyzed by ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry (UPLC-MS/MS) with an external standard. The detection method was a multiple reaction monitoring (MRM). And the effects of pH, elution solvent, and the amount of elution solvent on the extraction effect were investigated. The experimental quantitative analysis adopted the external standard method. The four fungicides displayed a good linear relationship in the concentration range of 0.10~50.0 μg/L, the detection limit was 0.004~0.095 μg/L, the recoveries were 68.7%~95.4%, and the relative standard deviations (n=5) were less than 10%. Using the method to detect fungicides is simple, fast, accurate, and sensitive.