Department Cell Toxicology, Helmholtz Centre for Environmental Research-UFZ, 04318, Leipzig, Germany.
Environmental Toxicology, Centre for Applied Geoscience, Eberhard Karls University Tübingen, 72074, Tübingen, Germany.
Anal Bioanal Chem. 2020 Oct;412(26):7295-7305. doi: 10.1007/s00216-020-02864-6. Epub 2020 Aug 15.
Solvent extracts of mammalian tissues and blood contain a large amount of co-extracted matrix components, in particular lipids, which can adversely affect instrumental analysis. Clean-up typically degrades non-persistent chemicals. Alternatively, passive sampling with the polymer polydimethylsiloxane (PDMS) has been used for a comprehensive extraction from tissue without altering the mixture composition. Despite a smaller fraction of matrix being co-extracted by PDMS than by solvent extraction, direct analysis of PDMS extracts was only possible with direct sample introduction (DSI) GC-MS/MS, which prevented co-extracted matrix components entering the system. Limits of quantitation (LOQ) ranged from 4 to 20 pg μL ethyl acetate (PDMS extract) for pesticides and persistent organic pollutants (POPs). The group of organophosphorus flame retardants showed higher LOQs up to 107 pg μL due to sorption to active sites at the injection system. Intraday precision ranged between 1 and 10%, while the range of interday precision was between 1 and 18% depending on the analyte. The method was developed using pork liver, brain, and fat as well as blood and was then applied to analyze human post-mortem tissues where polychlorinated biphenyls (PCBs) as well as dichlorodiphenyltrichloroethane (DDT) and DDT metabolites were detected. Graphical abstract.
哺乳动物组织和血液的溶剂提取物中含有大量共提取的基质成分,特别是脂质,这可能会对仪器分析产生不利影响。通常,净化会降解非持久性化学品。或者,使用聚合物聚二甲基硅氧烷(PDMS)进行被动采样,可以在不改变混合物组成的情况下从组织中进行全面提取。尽管 PDMS 共提取的基质部分比溶剂提取少,但只有使用直接进样(DSI)GC-MS/MS 才能直接分析 PDMS 提取物,这可以防止共提取的基质成分进入系统。农药和持久性有机污染物(POPs)的 PDMS 提取物的定量下限(LOQ)范围为 4 至 20 pg μL 乙酸乙酯。由于吸附到注射系统的活性位点,有机磷阻燃剂的 LOQ 更高,高达 107 pg μL。日内精密度在 1%至 10%之间,而日间精密度范围在 1%至 18%之间,具体取决于分析物。该方法使用猪肝、脑和脂肪以及血液进行开发,然后应用于分析人死后组织,其中检测到多氯联苯(PCBs)以及滴滴涕(DDT)和 DDT 代谢物。