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Evaluation of different scan methods for the urinary detection of corticosteroid metabolites by liquid chromatography tandem mass spectrometry

机译:液相色谱串联质谱法评估尿液中糖皮质激素代谢物的不同扫描方法的评价

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摘要

Different approaches for the non-target detection of corticosteroids in urine have been evaluated. As a result of previous studies about the ionization (positiveegative) and fragmentation of corticosteroids, several methods based on both precursor ion (PI) and neutral loss (NL) scans are proposed. The applicability of these methods was checked by the injection of a standard solution containing 19 model compounds. Five of the studied methods (NL of 76 Da; PI of 77, 91 and 105; PI of 237; PI of 121,147 and 171; and NIL of 38 Da) exhibited satisfactory results at the concentration level checked (corresponding to 20 ng/ml in sample). Some other methods in negative ionization mode such as the NIL of 104 Da were found to lack sufficient sensitivity. Some of the applied methods were found to be specific for a concrete structure (NL of 38 Da for fluorine containing corticosteroids) while others showed a wide range applicability (PI of 77, 91 and 105 showed response in all model compounds). interference by endogenous compounds was also tested by the analysis of negative urines and urines spiked with different corticosteroids. The suitability of these methods for the detection of corticosteroid metabolites was checked by the analysis of urine samples collected after the administration of methylprednisolone and triamcinolone. A combination of the reported methods seems to be the approach of choice in order to have a global overview about the excreted corticosteroid metabolites.
机译:已经评估了用于尿液中皮质类固醇非目标检测的不同方法。作为先前对皮质类固醇的电离(正/负)和碎片化研究的结果,提出了几种基于前体离子(PI)和中性损失(NL)扫描的方法。这些方法的适用性通过注入包含19种模型化合物的标准溶液进行检查。在所检查的浓度水平(相当于20 ng / ml)中,有5种研究方法(NL为76 Da; PI为77、91和105; PI为237; PI为121,147和171; NIL为38 Da)显示出令人满意的结果。样本中)。发现其他一些负电离模式的方法(如104 Da的NIL)缺乏足够的灵敏度。已发现某些应用的方法对混凝土结构是特定的(含氟皮质类固醇的NL为38 Da),而另一些方法则显示出广泛的适用性(所有模型化合物的PI为77、91和105)。还通过分析阴性尿液和掺入不同皮质类固醇的尿液测试了内源性化合物的干扰。通过分析甲基强的松龙和曲安西龙后收集的尿液样品,检查了这些方法对皮质类固醇代谢物检测的适用性。为了对分泌的皮质类固醇代谢物有一个整体的了解,似乎是已报道方法的组合。

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