摘要
建立了分散固相萃取-分散液液微萃取与高效液相色谱/质谱联用同时测定荔枝或香蕉中痕量氟硅唑、戊唑醇和烯唑醇3种农药残留的新方法.分散固相萃取方法以乙腈为萃取液,以N-丙基-乙二胺(PSA)和C18为吸附剂.对影响分散液液微萃取萃取效率的因素,如萃取溶剂种类及体积、分散剂、萃取时间等进行了优化.在最佳实验条件下,3种农药的线性范围为0.01～10μg/mL(r2≥0.999 7).在2种样本中添加不同质量浓度的目标分析物其平均回收率在73.6%～106.3%,相对标准偏差(n=6)小于3.8%,检出限为0.995～1.22μg/kg.用于实际样品中氟硅唑、戊唑醇和烯唑醇3种农药残留分析获得满意结果.
A novel method using dispersive solid-phase extraction （DSPE） and dispersive liquid-liquid mi- cro-extraction （DLLME） by high performance liquid chromatography-tandem mass spectrometry （HPLC MS/MS） was established for the determination of the residues of three pesticides in litchi and banana fruits. With dispersive solid-phase extraction, PSA and C18 were used as the sorbents and acetonitrile as the eluted solvent. Some experimental parameters that influence the extraction efficiency, such as the type and volume of the dispersive solvents and extraction solvents, extraction time, pH and salt addition, were examined and optimized. Under the optimum conditions, the linear ranges of the three insecticides were 0.010--10 p^g/mL, re^0.999 7. The method provided an acceptable accuracy （73.6 ~ 106.8 ~ recov- ery） and precision （43.8 Y00 relative standard deviation） for two samples with the limits of detection （S/N 3） ranging from 0. 995 to 1.22 ffg/kg. The proposed method has been successfully applied to the analy sis of the residues of flusilazole, tebuconazole and diniconazole in fruit samples with satisfactory results.
出处
《西南大学学报（自然科学版）》
CAS
CSCD
北大核心
2013年第5期102-106,共5页
Journal of Southwest University(Natural Science Edition)
基金
国家自然科学基金资助项目(21277110)
关键词
分散固相萃取
分散液液微萃取
高效液相色谱-质谱
农药残留
dispersive solid-phase extraction
dispersive liquid-liquid micro-extraction
HPLC-MS/MS
pesticide residue
