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. DOI: 10.16801/j.issn.1008-7303.2017.0029
    引用本文: 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. DOI: 10.16801/j.issn.1008-7303.2017.0029
    ZHAO Hua, WU Min, HE Hongmei, ZHANG Chunrong, HU Xiuqing, ZHANG Changpeng. Determination of zinc-thiazole residues in water, soil and Cucumis sativus L. by high performance liquid chromatography[J]. Chinese Journal of Pesticide Science, 2017, 19(2): 217-222. DOI: 10.16801/j.issn.1008-7303.2017.0029
    Citation: ZHAO Hua, WU Min, HE Hongmei, ZHANG Chunrong, HU Xiuqing, ZHANG Changpeng. Determination of zinc-thiazole residues in water, soil and Cucumis sativus L. by high performance liquid chromatography[J]. Chinese Journal of Pesticide Science, 2017, 19(2): 217-222. 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: 建立了采用高效液相色谱-二极管阵列检测器(HPLC-DAD)测定水、土壤和黄瓜中噻唑锌残留的方法。在碱性条件下先将噻唑锌转化为噻二唑(AMT),采用外标法通过测定噻二唑的量来进行噻唑锌的定量分析。样品在40℃恒温振荡条件下,依次经Na2S转化及乙腈提取;过滤后调节混合液pH值至3,经乙酸乙酯液-液分配后,用HPLC-DAD及BDS Hypersil-C18色谱柱,以V(乙腈):V(0.1%乙酸)=10:90为流动相,在313 nm波长下测定样品中的噻唑锌残留。结果表明:噻二唑在0.10~10 mg/L、噻唑锌在0.20~5.0 mg/L的质量浓度范围内线性关系良好(R2 > 0.999 5),噻二唑的检出限(LOD)为0.05 mg/L。在0.2、1和5 mg/L添加水平下,噻唑锌在水中的平均回收率为100%~110%,相对标准偏差(RSD)为0.90%~6.4%;在0.05、0.5和5 mg/kg添加水平下,噻唑锌在土壤中的平均回收率为81%~98%,RSD为0.70%~2.8%;在0.05、0.5和2 mg/kg添加水平下,噻唑锌在黄瓜中的平均回收率为95%~102%,RSD为1.3%~4.2%。噻唑锌在水、黄瓜和土壤中的定量限(LOQ)分别为0.03 mg/L、0.05 mg/kg和0.05 mg/kg。本方法简单、准确、可靠,能满足农药残留分析的要求。

       

      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 0.999 5. 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.

       

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