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周添, 刘菲. 小体积液液萃取气相色谱-质谱法测定地下水中的克百威与3-羟基克百威[J]. 岩矿测试, 2021, 40(3): 358-364. DOI: 10.15898/j.cnki.11-2131/td.202009050122
引用本文: 周添, 刘菲. 小体积液液萃取气相色谱-质谱法测定地下水中的克百威与3-羟基克百威[J]. 岩矿测试, 2021, 40(3): 358-364. DOI: 10.15898/j.cnki.11-2131/td.202009050122
ZHOU Tian, LIU Fei. Determination of Carbofuran and 3-Hydroxycarbofuran in Groundwater by Small Volume Liquid-Liquid Extraction Combined with GC-MS[J]. Rock and Mineral Analysis, 2021, 40(3): 358-364. DOI: 10.15898/j.cnki.11-2131/td.202009050122
Citation: ZHOU Tian, LIU Fei. Determination of Carbofuran and 3-Hydroxycarbofuran in Groundwater by Small Volume Liquid-Liquid Extraction Combined with GC-MS[J]. Rock and Mineral Analysis, 2021, 40(3): 358-364. DOI: 10.15898/j.cnki.11-2131/td.202009050122

小体积液液萃取气相色谱-质谱法测定地下水中的克百威与3-羟基克百威

Determination of Carbofuran and 3-Hydroxycarbofuran in Groundwater by Small Volume Liquid-Liquid Extraction Combined with GC-MS

  • 摘要: 克百威和3-羟基克百威是一对典型的农药母体及其代谢产物,由于其水溶性高、毒性大,可通过地表水或地下水进行长距离迁移,对人类健康和环境安全造成危害。以往通常采用液相萃取或固相萃取的方式提取样品中的克百威和3-羟基克百威,但这些方法操作繁琐、耗时较长,不利于室内模拟实验中多组样品的检测。为实现克百威与3-羟基克百威在地下水中的快速定量,本文建立了一种小体积液液萃取的前处理方法进行提取,并采用气相色谱-质谱(GC-MS)进行检测,对影响克百威和3-羟基克百威萃取效率的因素进行了研究。通过实验对比不同萃取剂、不同pH、不同离子强度条件下克百威与3-羟基克百威的回收率,优化了前处理条件。结果表明,选择二氯甲烷作为萃取剂且用量为1mL,调节水样pH=5,氯化钠用量为40g/L时克百威和3-羟基克百威的回收率最高,分别为75.1%~98.6%、55.0%~66.3%。性能评价结果显示,方法精密度和方法准确度满足测试要求(相对标准偏差 < 10%,n=5),克百威和3-羟基克百威的方法检出限分别为15.3μg/L、10.2μg/L。该方法操作简便、快速、消耗溶剂少,与传统的液液萃取法相比,本方法耗时约为前者的1/8,消耗溶剂量约比前者小2个数量级,能够满足室内模拟实验需求。

     

    Abstract:
    BACKGROUNDCarbofuran and 3-hydroxycarbofuran are typical pesticides with the relationship of parent and metabolite. Due to high water solubility and toxicity, carbofuran and 3-hydroxycarbofuran can be transported through surface water or groundwater for long distances, causing harm to human health and environmental safety. In the past, carbofuran and 3-hydroxycarbofuran in samples were usually extracted by liquid or solid phase extraction. However, these methods are cumbersome to operate and time-consuming, which is not conducive to the detection of multiple sets of samples in indoor simulation experiments.
    OBJECTIVESIn order to realize the rapid quantification of carbofuran and 3-hydroxycarbofuran in groundwater.
    METHODSA small volume liquid-liquid extraction pretreatment method was established for extraction, combined with gas chromatography-mass spectrometry to detect factors affecting the extraction efficiency of carbofuran and 3-hydroxycarbofuran. To improve the extraction efficiency of carbofuran and 3-hydroxycarbofuran, JP factors such as the type of extraction solvent, pH and dosage of NaCl were optimized.
    RESULTSResults showed that the extraction efficiency of carbofuran and 3-hydroxycarbofuran was highest when 1mL methylene chloride was selected as the extraction agent under pH=5, and 40g/L NaCl was added in the water samples. The extraction recoveries for carbofuran and 3-hydroxycarbofuran were 75.1%-98.6% and 55.0%-66.3%, respectively. The performance evaluation results showed that the instrument precision and method precision meet test requirements (n=5, relative standard deviation < 10%). The detection limits of carbofuran and 3-hydroxycarbofuran in water were 15.3μg/L and 10.2μg/L, respectively.
    CONCLUSIONSThis method is simple and fast with less solvent. Compared with the traditional liquid-liquid extraction method, this method takes about 1/8 time of the former, and consumes about two orders of magnitude less solvent than the former, which can meet the needs of indoor simulation experiments.

     

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