建立了一种固相萃取(SPE)前处理,高效液相色谱/质谱联用分析(HPLC/MS)测定水体中痕量新烟碱类杀虫剂(啶虫脒、噻虫胺、呋虫胺、吡虫啉、噻虫啉和噻虫嗪)含量的方法.确立HPLC/MS分析方法,并采用响应曲面法中Box-Behnken实验设计优化了SPE的吸附剂类型和用量、洗脱液类型和用量,获得以100 mgHLB为吸附剂及10 mL甲醇为洗脱液的前处理方法.所建方法适用于分析水中较宽浓度范围(3个数量级:0.9-100 ng·mL-1)的新烟碱类杀虫剂,回收率范围为75.4％±0.98％—122％±1.7％.此外,目标物的方法检测限均低于3 ng·L-1,相对标准偏差范围为2.99％-7.92％,低于文献值,说明所建方法具有较好的灵敏度和精密度.最后,该方法成功用于分析野外采集的水样,验证了该方法分析环境水体中新烟碱类杀虫剂的适用性.
An method has been established for determining trace neonicotinoid insecticides (acetamiprid,clothianidin,dinotefuran,imidacloprid,thiacloprid and thiamethoxa) in water using high performance liquid chromatography/mass spectrometry (HPLC/MS) after sample preparation with solid phase extraction (SPE).After setting up HPLC-MS method,response surface methodology (Box-Behnken design) was applied to select the type and mass of sorbents and the type and volume of elution solution for SPE.The optimized SPE method used 100 mg HLB as the sorbent and 10 mL methanol as the elution solvent.The newly developed method was validated by analyzing target insecticides in water in a wide range of concentrations (up to three multitudes:0.9 ng·L-1-100 ng·mL-1),and the recovery of analytes ranged from (75.4±0.98) ％ to (122± 1.7) ％.The method detection limits for all neonicotinoids were less than 3 ng· L-1 with the relative standard deviations from 2.99％ to 7.92％.The values were lower than those in previous studies,indicating good sensitivity and precision of the established method.Eventually,the method was successfully applied to determine neonicotinoids in field water samples,validating the effectiveness of the newly developed method in the environment.
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