Greulich Kerstin, Alder Lutz
Federal Insitute for Risk Assessment, P.O. Box 330013, 14191, Berlin, Germany.
Anal Bioanal Chem. 2008 May;391(1):183-97. doi: 10.1007/s00216-008-1935-x. Epub 2008 Mar 3.
The study tested the determination of 300 pesticides in mineral water at levels of 0.1 and 1.0 microg/L. Measurements were conducted by direct sample injection into a liquid chromatograph coupled to a tandem mass spectrometer without any sample enrichment and/or cleanup. Two separate injections enabled the recording of two transitions per analyte (600 selected reaction monitoring transitions in total). For 285 analytes the sensitivity of direct sample injection (100 microL) was sufficient to quantify residues at 0.1 microg/L. All remaining pesticides were detected at 1.0 microg/L. Calibration functions were linear for more than 80% of analytes. Signal suppression or enhancement compared with signals in high-performance liquid chromatography water was equal to or smaller than 20% for 240 analytes. Even the largest matrix-induced suppression did not result in the disappearance of peaks. Combining the results of seven mineral waters, the relative standard deviation of "recovery" was 20% or less for 87% of the substances. A second transition for confirmatory purposes was often available. Consequently, the proposed direct injection of samples without any sample enrichment and/or cleanup is suitable for screening of many pesticides in mineral and drinking water.
该研究检测了矿泉水中300种农药在0.1和1.0微克/升水平下的含量。通过直接将样品注入与串联质谱仪联用的液相色谱仪进行测量，无需任何样品富集和/或净化。两次单独进样可记录每种分析物的两个跃迁（总共600个选择反应监测跃迁）。对于285种分析物，直接进样（100微升）的灵敏度足以定量0.1微克/升的残留。所有其余农药在1.0微克/升时被检测到。超过80%的分析物校准函数呈线性。与高效液相色谱水中的信号相比，240种分析物的信号抑制或增强等于或小于20%。即使最大的基质诱导抑制也不会导致峰消失。综合七种矿泉水的结果，87%的物质“回收率”的相对标准偏差为20%或更低。通常有用于确证目的的第二个跃迁。因此，所提出的无需任何样品富集和/或净化的直接进样适用于矿泉水中和饮用水中多种农药的筛查。
