| 高效液相色谱法测定噻唑锌在水、土壤及黄瓜中的残留 |
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| 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. |
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| 作者姓名： | 赵华 吴珉 何红梅 张春荣 胡秀卿 张昌朋 |
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| 作者单位： | 1.浙江省农业科学院 农产品质量标准研究所/省部共建国家重点实验室培育基地"浙江省植物有害生物防控重点实验室"/农业部农药残留检测重点实验室, 杭州 310021 |
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| 基金项目： | 农业部农业行业标准制定项目（2130109）. |
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| 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。
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| 关 键 词： | 高效液相色谱 噻唑锌 水 土壤 黄瓜 残留 |
| 收稿时间： | 2016/8/22 0:00:00 |
Determination of zinc-thiazole residues in water, soil and Cucumis sativus L. by high performance liquid chromatography |
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| ZHAO Hu,WU Min,HE Hongmei,ZHANG Chunrong,HU Xiuqing and 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. |
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| Authors: | ZHAO Hu WU Min HE Hongmei ZHANG Chunrong HU Xiuqing and ZHANG Changpeng |
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| Institution: | 1.State Key Laboratory Breeding Base for Zhejiang Sustainable Plant Pest Control/Ministration of Agriculture Key Laboratory for Pesticide Residue Detection/Institute of Quality and Standard for Agro-products, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, China |
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| 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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| Keywords: | high performance liquid chromatography zinc-thiazole water soil Cucumis sativus L residue |
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