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Ultratrace analysis of atrazine in soil using Ice Concentration Linked with Extractive Stirrer and High Performance Liquid Chromatography—Tandem Mass Spectrometry
Journal of Chromatography A ( IF 4.1 ) Pub Date : 2020-11-27 , DOI: 10.1016/j.chroma.2020.461753
Christopher S. Skaggs , Brian A. Logue

Atrazine is a widely-used pesticide with a relatively long half-life in the environment. This leads to persistent soil contamination with the potential of migration to ground and surface waters. Analysis of atrazine in soil is difficult due to the inherent complexity of soil as a sample matrix. Moreover, the moderate hydrophobicity of atrazine makes it difficult to extract into typical sorbent phases during sample preparation. Therefore, a method for the ultratrace determination of atrazine in soil using Ice Concentration Linked with Extractive Stirrer (ICECLES) and high performance liquid chromatography—tandem mass spectrometry (HPLC-MS/MS) was developed to address these issues. For the method, soil samples (10 g) were initially extracted with methanol:water (8:2, v:v), followed by solvent exchange to 100% water. The samples then underwent ICECLES with back-extraction into 100% methanol prior to HPLC-MS/MS analysis. The ICECLES-HPLC-MS/MS method produced a wide linear range of 10 to 1000 ng/kg, featured excellent limits of quantification and detection of 10 and 5 ng/kg, respectively, and good accuracy (100 ± 12%) and precision (≤9.6% relative standard deviation). This method was tested on field soil samples and provided ultratrace detection of atrazine. With this method, previously unachievable low parts per trillion (ppt) detection of atrazine in soil is now possible.



中文翻译:

萃取搅拌器与高效液相色谱-串联质谱联用的冰浓度超痕量分析土壤中的阿特拉津

阿特拉津是一种广泛使用的农药,在环境中具有相对较长的半衰期。这导致土壤持续污染,并可能迁移到地下水和地表水中。由于土壤固有的复杂性,很难对土壤中的去津进行分析。此外,at去津的适度疏水性使其在样品制备过程中难以提取到典型的吸附相中。因此,为解决这些问题,开发了一种使用萃取搅拌器(ICECLES)和冰浓度联合高效液相色谱-串联质谱法(HPLC-MS / MS)测定土壤中阿特拉津的超痕量方法。对于该方法,首先用甲醇:水(8:2,v:v)提取土壤样品(10 g),然后将溶剂交换为100%的水。然后在进行HPLC-MS / MS分析之前,先对样品进行ICECLES,然后反萃取至100%甲醇中。ICECLES-HPLC / MS / MS方法产生的线性范围为10到1000 ng / kg,定量和检出限分别为10 ng / kg和5 ng / kg,具有出色的准确度(100±12%)和精度(相对标准偏差≤9.6%)。该方法在田间土壤样品上进行了测试,并提供了阿特拉津的超痕量检测。通过这种方法,现在可以实现以前无法实现的土壤中阿特拉津的低百亿分之几(ppt)检测。相对标准偏差的6%)。该方法在田间土壤样品上进行了测试,并提供了阿特拉津的超痕量检测。通过这种方法,现在可以实现以前无法实现的土壤中阿特拉津的低百亿分之几(ppt)检测。相对标准偏差的6%)。该方法在田间土壤样品上进行了测试,并提供了阿特拉津的超痕量检测。通过这种方法,现在可以实现以前无法实现的土壤中阿特拉津的低百亿分之几(ppt)检测。

更新日期:2020-12-04
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