摘要
利用超高效液相色谱建立了同时测定稻田土壤及水中噻虫啉、氟虫双酰胺及其代谢产物残留的快速分析方法。稻田水样以乙酸乙酯萃取,有机相经浓缩后定容;土壤样品用水润湿后以丙酮提取,液-液分配净化。优化的色谱条件为:采用ACQUITY UPLC HSS T3色谱柱(2.1 mm×100 mm,1.8μm)分离,以乙腈-水为流动相,流速0.3 mL.min-1,柱温35℃,进样量5μL,检测波长230 nm。结果表明,噻虫啉、氟虫双酰胺及其代谢产物在0.01～10.00 mg.L-1质量浓度范围内呈良好线性关系,相关系数分别为1.000、1.000、0.999 9;噻虫啉、氟虫双酰胺及其代谢产物的仪器测定限为0.001～0.002 mg.L-1,在稻田水中的方法检出限为0.000 4～0.001 0 mg.L-1,在土壤中的方法检出限为0.002 2～0.003 6 mg.kg-1;对稻田土壤及水中的噻虫啉、氟虫双酰胺及其代谢产物进行不同水平的加标回收率实验,得到方法的回收率为82%～106%,相对标准偏差(n=5)为0.81%～3.8%。该方法操作简便,分离效果好,灵敏度与准确度良好,已成功应用于实际样品的检测。
An ultra performance liquid chromatographic（UPLC） method was developed for the determination of thiacloprid,flubendiamide and their metabolite residues in paddy soil and water.The paddy water was extracted with ethyl acetate,and the organic phase was concentrated to constant.The paddy soil was extracted with acetone-water and the extract was purified by liquid-liquid distribution.The optimization chromatographic conditions were as the follows：separation column：ACQUITY UPLC HSS T3 chromatographic column（2.1 mm×100 mm,1.8 μm）,mobile phase：acetonitrile-water,flow rate：0.3 mL·min-1,column temperature：35 ℃,sample volume：5 μL,detection wavelength：230 nm.Under the optimized conditions,the calibration curves of thiacloprid,flubendiamide and their metabolite residues showed good linearities in the range of 0.01-10.00 mg·L-1 with correlation coefficients of 1.000,1.000,0.999 9,respectively.The instrumental detection limits of three compounds were in the range of 0.001-0.002 mg·L-1,and their method detection limits were 0.000 4-0.001 0 mg·L-1 for water sample and 0.002 2-0.003 6 mg·kg-1 for soil sample.The spiked recoveries were in the range of 82%-106% with RSDs（n=5） of 0.81%-3.8%.With the advantages of easy operation,good separation effect,high sensitivity and accuracy,the proposed method was successfully applied in the determination of thiacloprid,flubendiamide and their metabolites in real samples.
出处
《分析测试学报》
CAS
CSCD
北大核心
2013年第1期138-142,共5页
Journal of Instrumental Analysis
基金
中央级公益性科研院所基本科研业务费专项
关键词
噻虫啉
氟虫双酰胺
稻田土壤
稻田水
超高效液相色谱
残留
thiacloprid
flubendiamide
paddy soil
paddy water
ultra performance liquid chro-matography （ UPLC ）
residue
