气相色谱-质谱法结合QuEChERS方法和分散液液微萃取技术测定茭白中三唑类农药残留  

Determination of Triazole Pesticides in Zizania Latifolia by GC-MS Combined with QuEChERS and Dispersive Liquid-Liquid Microextraction

作　　者：姚芳[1] 宋志宇[1] 聂晶[1] 叶静青 韦其真 倪琳[1] 李祖光[1] 

机构地区：[1]浙江工业大学化学工程学院,杭州310014

出　　处：《理化检验（化学分册）》2017年第6期650-654,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：浙江省自然科学基金项目(LY16B050008);浙江省科技厅公益项目(2015C32006);浙江省植物有害生物防控重点实验室资助项目(2010DS700124-KF1701);杭州市钱江特聘专家项目(2014)

摘　　要：采用QuEChERS方法结合分散液液微萃取技术萃取茭白中的腈菌唑、戊唑醇和苯醚甲环唑残留,并采用气相色谱-质谱法进行测定。3.000g样品经3mL乙腈超声提取1min,提取液经30mg的PSA与30mg的C_(18)混合吸附剂净化。移取800μL净化液于巴斯德吸管中,加入甲苯30μL,混匀后快速注入水2.5mL,超声45s后离心,上层有机相经无水硫酸钠除水后在DB-5MS毛细管色谱柱上分离,质谱分析中选择电子轰击离子源和选择离子监测模式。3种农药的线性范围分别为5.0~500,5.0~500,12.5~1 250μg·kg^(-1),检出限(3S/N)分别为1.4,0.86,3.0μg·kg^(-1)。加标回收率为82.7%~116%,测定值的相对标准偏差(n=5)为4.1%~15%。The residues of myclobutanil, tebuconazole and dKenoconazole in Zizania latifolia were extracted with a method of QuEChERS combined with dispersive liquid-liquid microextraetion （DLLME）, and then determined by GCMS. The sample （3. 000 g） was ultrasonically extracted with 3 mL of acetonitrile for 1 min, and the extract was cleaned up with a mixture of PSA （30 mg） and C18 （30 mg）. The purified solution （800 μL） was transferred to Pasteur pipette, and then 30μL of toluene was added. After the solution was mixed well, 2.5 mE of water was injected quickly and the solution was treated with ultrasonic for 45 s and centrifugation. After dehydration with anhydrous sodium sulfate, the upper organic phase was separated on a DB-5MS capillary chromatographic column. EI and SIM were adopted in MS analysis. The linearity ranges of the 3 presticides were 5.0--500, 5.0-- 500, 12.5--1 250 μg · kg^-1 respectively, with detection limits of 1.4, 0.86, 3.0μg · kg^- 1 respectively. Recovery rates obtained by standard addition method were 82.7%-116%, and RSDs （n=5） were 4. 1%-15%.

关 键 词：QuEChERS 分散液液微萃取 气相色谱-质谱法 腈菌唑 戊唑醇 苯醚甲环唑 

分 类 号：O657.63[理学—分析化学]