| 摘要: |
| [目的]为检测水体及其他流体中毒死蜱及其降解物3,5,6-三氯吡啶-2-酚(TCP)残留提供简便而准确的分析方法.[方法]对固相萃取水样的pH、洗脱剂,以及高效液相色谱的流动相组成、pH、梯度洗脱条件、最佳检测波长进行了筛选,建立了环境水体中毒死蜱及其降解产物TCP的固相萃取-高效液相色谱法,并用该方法检测了10份不同来源水样中毒死蜱和TCP的质量浓度.[结果]建立的固相萃取-高效液相色谱法为:水体样品先用5 mol/L盐酸调pH为4.5,过滤后取1 L滤过液经固相萃取(SPE)小柱提取、净化,用二氯甲烷-丙酮-乙腈混合液(V(二氯甲烷):V(丙酮):V(乙腈)=40:60:20)洗脱,然后用乙腈-超纯水(pH 3.5)梯度洗脱法对毒死蜱和TCP进行分离,于波长为230 nm下用二极管阵列检测器(DAD)检测,外标法定量.该方法对毒死蜱和TCP的检出限分别为0.15 mg/L和0.30 mg/L,最小检出质量浓度均为0.001 mg/L,线性范围均为0.3～10 mg/L,添加回收率均在70%以上,相对标准偏差分别为0.7%～13.0%和2.7%～7.8%.用该方法测定了不同来源的10份水样,结果可靠.[结论]建立的固相萃取-高效液相色谱法灵敏度、准确度和精密度完全可以满足水体中毒死蜱和TCP残留检测要求,亦为其他流体中毒死蜱及TCP分析提供了参考. |
| 关键词: 固相萃取 高效液相色谱 毒死蜱 3,5,6-三氯吡啶-2-酚 水样 |
| DOI： |
| 分类号:F301 |
| 基金项目:科技部科技成果转化项目（05EFN214400207）；广东省自然科学基金项目(05006634)；广东省教育厅自然科学研究项目(04020615)；广州市科学技术局资助项目（2005Z2-E0061） |
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| Determination of chlorpyrifos and its metabolite in water samples by solid-phase extraction and high performance liquid chromatography |
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WU Cheng-liang LIU Jun-chang BAO Qing-feng SU Yin-quan
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| Abstract: |
| 【Objective】 The aim of the present work was to provide a simple and exact analytical method to determine chlorpyrifos and its main metabolite 3,5,6-trichloro-2-pyridinol（TCP）in environmental water and the other fluid.【Method】 To study the pH in water sample,eluting solvents in SPE,and the pH in mobile phase,the condition of gradient elution for HPLC,and the best checking wavelength of chlorpyrifos and TCP,an analytical method for determination of chlorpyrifos and its main metabolite TCP in environmental water by solid-phase extraction (SPE) coupled with high performance liquid chromatography（HPLC）with diode-array detector（DAD）was developed.The concentrations of chlorpyrrfos and TCP in ten water samples collecting different sites were determined by this method. 【Result】 The method was:the water samples were acidified with 5 mol/L acetic acid (pH 4.5),then filtrated.1 L of filtrate was extracted and purified using solid phase extraction, and eluted with dichloromethane,the mixture of acetone-acetonitrile (V（dichloromethane）∶V（acetone）∶V（acetonitrile）=40∶60∶20).The Chlorpyrifos and TCP were separated with acetonitrile/water (pH 3.5) under the condition of gradient elution,measured by DAD at 230 nm,the external standard method was used for quantification.The limits of detection were 0.15 mg/L and 0.30 mg/L for chlorpyrifos and TCP,respectively,the LOQ of chlorpyrifos and TCP are 0.001 mg/L,the linear range is 0.30－10 mg/L.The fortified recoveries of chlorpyrifos and TCP were above 70% for environmental water,with relative standard deviations of 0.7%－13.0% and 2.7%-7.8%,respectively.This method is applied to detect chlorpyrifos and TCP in 10 samples of environmental water collected from different sites.The results are reliable. 【Conclusion】 It is a sensitive,simple and reliable method and the recovery rate and coefficient of variation are perfect.The method suited the demand of detecting the chlorpyrifos and TCP in the environmental waters,also provided a reference of analyzing the concentrations of chlorpyrifos and TCP in the other liquid. |
| Key words: solid phase extraction high performance liquid chromatography chlorpyrifos 3,5,6-trichloro-2-pyridinol water sample |
