农药学学报2017，Vol.19Issue(2)：217-222,6.DOI:10.16801/j.issn.1008-7303.2017.0029
高效液相色谱法测定噻唑锌在水、土壤及黄瓜中的残留
Determination of zinc-thiazole residues in water, soil and Cucumis sativus L. by high performance liquid chromatography
摘要
Abstract
A new residue determination method for zinc-thiazole in water, soil and Cucumis sativus L. samples has been developed and validated by high performance liquid chromatography with diode array detection. Zinc-thiazole (bis-(2-amino-5-mercapto-1,3,4-thiadiazole)zinc) was converted into AMT (2-amino-5-mercapto-1,3,4-thiadiazole) in the alkaline solution. The quantitative analysis of zinc-thiazole was then achieved by the determination of AMT. Samples were reacted with sodium sulfide, and extracted with acetonitrile at 40 ℃. The mixture was filtered and the pH of the filtrate was adjusted to 3. The filtrate clean-up was conducted by liquid-liquid extraction (LLE) using ethyl acetate. The determination was carried out using HPLC-DAD (313 nm) with BDS Hypersil C18 column and V (acetonitrile) : V (0.1% acetic acid) = 10 : 90 were used as the mobile phase. The analyte was quantified by external standard method. The results showed that the linear range of this method was 0.1-10 mg/L for AMT, 0.2-5 mg/L for zinc-thiazole. And the correlation coefficients were above 0.9995. The limits of detection (LODs) for AMT was 0.05 mg/L. The average recovery of zinc-thiazole in water, soil and C. sativus at three spiked levels (0.05-5 mg/kg) were 81%-110% with relative standard deviations (RSDs, n=5) ranged from 0.7% to 6.4%. The limit of quantification (LOQs) of zinc-thiazole in water, C. sativus and soil samples were 0.03, 0.05 and 0.05 mg/kg, respectively. This method is simple, accurate and reliable, which is suitable for the determination of zinc-thiazole in water, soil and C. sativus.关键词
高效液相色谱/噻唑锌/水/土壤/黄瓜/残留Key words
high performance liquid chromatography/zinc-thiazole/water/soil/Cucumis sativus L/residue分类
农业科技引用本文复制引用
赵华,吴珉,何红梅,张春荣,胡秀卿,张昌朋..高效液相色谱法测定噻唑锌在水、土壤及黄瓜中的残留[J].农药学学报,2017,19(2):217-222,6.基金项目
农业部农业行业标准制定项目(2130109). （2130109）
