liquid chromatography - triple quadrupole mass spectrometer (LC-MS/MS)

用于小极性分子（真菌毒素、生理代谢物、食品成分、污染物、药剂、信号分子等）的高灵敏度和选择性痕量分析和定量。在复杂的生物基质中（食品样品、生理样品、细胞培养样品、组织样品、药用植物、昆虫等）（超）高效液相色谱-串联质谱联用（（U）HPLC-MS / MS）是首选方法。食品-化学-毒理学背景下以及药物-生物学问题中的许多分子关系只能在体外或体内复杂的测试系统中回答。特别是对于强效污染物或活性物质，这意味着通常必须分析极低浓度才能获得有意义的数据。例如，如果必须对单个细胞隔室中的分析物含量进行定量，或者必须通过其产生谱来表征代谢物，则对分析系统的性能的要求进一步增加。在人体生物监测领域，对检测限和定量限的要求也极高，因为必须在生理样本中测定霉菌毒素及其代谢物等污染物的最低浓度，以便能够有意义地确定人体接触情况。在使用真菌毒素生物监测的队列研究中，这意味着左删失数据的数量，即水平低于检测限的分析结果，基本上决定了观察到的关系和影响变量的重要性。同时，队列规模对于干预研究的信息价值也至关重要。这里应该提到几千份尿样的SHINE研究作为一个例子，使用这些数量级的复杂样品制备是不可能的。为此，应用了与UHPLC系统和在线固相萃取连接的高灵敏度三重四极杆质谱仪。通过离子阱（QTRAP）的额外进一步碎片化可能性也旨在实现更高的选择性，并且还可以在最低浓度范围内生成生产光谱，以更好地表征未知代谢物。

For the highly sensitive and selective trace analysis and quantification of small polar molecules (mycotoxins, physiological metabolites, food ingredients, contaminants, pharmaceutical agents, signal molecules, etc.) in complex biological matrices (food samples, physiological samples, cell culture samples, tissue samples, medicinal plants, insects, etc.) the coupling of (ultra) high-performance liquid chromatography with tandem mass spectrometry ((U) HPLC-MS / MS) is the method of choice. Many molecular relationships in the food-chemical-toxicological context but also in pharmaceutical-biological issues can only be answered in complex test systems in vitro or in vivo. In the case of potent contaminants or active substances in particular, this means that extremely low concentrations often have to be analyzed in order to obtain meaningful data. If, for example, the analyte content in individual cell compartments has to be quantified or metabolites have to be characterized by their production spectrum, the demands on the performance of the analytical system increase further. In the area of human biomonitoring, the requirements with regard to detection and quantification limit are also extremely high, since here the lowest concentrations of contaminants such as mycotoxins and their metabolites must be determined in physiological samples in order to enable a meaningful determination of human exposure. In cohort studies using the biomonitoring of mycotoxins, this means that the amount of left censored data, i.e. analytical results with levels below the detection limit, essentially determines the significance of the observed relationships and influencing variables. At the same time, the cohort size is also essential for the informative value of intervention studies. The SHINE study with several thousand urine samples should be mentioned here as an example, with these orders of magnitude complex sample preparations are not possible. For this reason, a highly sensitive triple quadrupole mass spectrometer in connection with a UHPLC system and online solid phase extraction is applied for. An additional further fragmentation possibility via an ion trap (QTRAP) is also intended to achieve increased selectivity, and it is also possible to generate production spectra in the lowest concentration range for better characterization of unknown metabolites.