Bünning Tobias Hartwig, Strehse Jennifer Susanne, Hollmann Ann Christin, Bötticher Tom, Maser Edmund
Institute of Toxicology and Pharmacology for Natural Scientists, University Medical School Schleswig-Holstein, Brunswiker Straße 10, 24105 Kiel, Germany.
Toxics. 2021 Mar 16;9(3):60. doi: 10.3390/toxics9030060.
To determine the amount of the explosives 1,3-dinitrobenzene, 2,4-dinitrotoluene, 2,4,6-trinitrotoluene, and its metabolites in marine samples, a toolbox of methods was developed to enhance sample preparation and analysis of various types of marine samples, such as water, sediment, and different kinds of biota. To achieve this, established methods were adapted, improved, and combined. As a result, if explosive concentrations in sediment or mussel samples are greater than 10 ng per g, direct extraction allows for time-saving sample preparation; if concentrations are below 10 ng per g, techniques such as freeze-drying, ultrasonic, and solid-phase extraction can help to detect even picogram amounts. Two different GC-MS/MS methods were developed to enable the detection of these explosives in femtogram per microliter. With a splitless injector, limits of detection (LODs) between 77 and 333 fg/µL could be achieved in only 6.25 min. With the 5 µL programmable temperature vaporization-large volume method (PTV-LVI), LODs between 8 and 47 fg/µL could be achieved in less than 7 min. The detection limits achieved by these methods are among the lowest published to date. Their reliability has been tested and confirmed by measuring large and diverse sample sets.
为了测定海洋样品中1,3-二硝基苯、2,4-二硝基甲苯、2,4,6-三硝基甲苯及其代谢物的含量,开发了一套方法工具包,以加强对各类海洋样品(如水、沉积物和不同种类生物群)的样品制备和分析。为此,对已有的方法进行了调整、改进和组合。结果表明,如果沉积物或贻贝样品中的爆炸物浓度大于每克10纳克,直接萃取可实现省时的样品制备;如果浓度低于每克10纳克,冷冻干燥、超声和固相萃取等技术有助于检测出甚至皮克级的含量。开发了两种不同的气相色谱-串联质谱法(GC-MS/MS),以实现对这些爆炸物在飞克每微升水平的检测。采用不分流进样器,仅需6.25分钟即可实现77至333飞克/微升的检测限(LOD)。采用5微升程序升温汽化-大体积进样法(PTV-LVI),在不到7分钟的时间内可实现8至47飞克/微升的检测限。这些方法所达到的检测限是迄今为止已发表的最低水平之一。通过对大量多样的样品集进行测量,测试并证实了它们的可靠性。