论文标题
可靠的LC-MS/MS基于基于痕量水平的方法,将50个培养基和高度极性农药残留在沉积物和生态风险评估中
Reliable LC-MS/MS-based method for trace level determination of 50 medium to highly polar pesticide residues in sediments and ecological risk assessment
论文作者
论文摘要
由于疏水性相对较差,在环境中的持久性显然较少,因此未广泛研究了沉积物中极性农药的发生。但是,它们的连续释放到水生系统中要求评估它们在沉积物中的潜在积累以及该基质作为这些化合物的潜在来源的作用。考虑到这一点,开发了一种基于加压液体提取(PLE)的方法,通过固相提取(SPE)(SPE)提取清理,并通过液相色谱测定分析物,并开发出与串联质谱法(LC-MS/MS)耦合的液相色谱法(LC-MS/MS),并经过验证,以分析50分析(经常使用和/或在水中经常使用和/或在水中发现或在水中发现的)。该方法在准确性(76%至124%之间的相对回收率),精度(相对标准偏差值<20%),灵敏度(大多数化合物的低Ng/g中的LOD),线性(确定> 0.99的系数)和MATRIX效果(所有分析可忽略的)方面表现出了良好的性能。使用同位素稀释方法进行定量确保结果可靠性。作为验证过程的一部分,该方法应用于Llobregat River(NE Spain)沉积物中靶农药的分析,显示了其中五个,即Terbutryn,Dichlorvos,Dichlorvos,Terbuthylazine,Terbuthylazine,diamzinon和Irgarol。由于发现的浓度及其物理化学特征,所有5种农药都表现出对水生生物的生物蓄积和风险的高潜力。需要研究不同水生室中农药发生并评估水生生态系统的潜在风险的其他多学科研究,以评估沉积物中农药存在的环境影响和重要性。
The occurrence of polar pesticides in sediments has not been extensively investigated because of their relatively poor hydrophobicity and apparently less persistence in the environment. However, their continuous release into the aquatic systems calls for the evaluation of their potential accumulation in sediments and the role of this matrix as a potential source of these compounds. Considering this, a method based on pressurized liquid extraction (PLE), extract clean-up by solid phase extraction (SPE) and analyte determination by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) was developed and validated to analyze 50 relevant (frequently used and/or regulated or found in water) medium to highly polar pesticides in sediments. The method showed good performance regarding accuracy (relative recoveries between 76% and 124%), precision (relative standard deviation values <20%), sensitivity (LODs in the low ng/g for most compounds), linearity (coefficients of determination >0.99), and matrix effects (negligible for all analytes). The use of an isotope dilution approach for quantification ensures results reliability. As a part of the validation process, the method was applied to the analysis of the target pesticides in sediments from the Llobregat River (NE Spain) showing the presence of five of them, namely, terbutryn, dichlorvos, terbuthylazine, diazinon, and irgarol. All 5 pesticides, due to both the concentrations found and their physical-chemical characteristics, demonstrate high potential for bioaccumulation and risk to the aquatic organisms. Additional multidisciplinary studies that investigate pesticides occurrence in the different aquatic compartments and evaluate the potential risks for aquatic ecosystems are required to assess the environmental impact and significance of the presence of pesticides in sediments.