An analytical technique was developed for the detection of phosphorus-containing compounds, using high-resolution-accurate-mass (HRAM) LC-MS. This method was constructed as a “flagging” approach for chromatographic peaks of compounds suspected of containing phosphorus, using high-energy in-source CID fragmentation, in parallel with a Full-MS experiment. Selective peak picking is achieved by tracking the highly resolved low m/z product ions of phosphorus-containing products, indicative of several phosphate and phosphonate groups. The chemical formula is then specifically assigned by a simultaneous accurate mass measurement of the precursor ion, together with the confirmed presence of a phosphorus atom in the suspect peak. This new method is demonstrated with various phosphorus-containing compounds such as V-class chemical warfare agents, nerve agents’ degradation products, pesticides, organic phosphates and a phospholipid. For these compounds, the developed method was found to be effective at concentrations as low as 1 ng/mL, in environmental extracts of soil and in urine (in the case of the phospholipid), making it comparable to selective phosphorus detectors such as GC-FPD, but with a much broader scope for charged, polar, or larger compounds.

开发了一种分析技术，该技术使用高分辨率精确质量（HRAM）LC-MS检测含磷化合物。该方法被构造为“旗标”方法，使用高能源CID裂解技术与涉嫌含磷化合物的色谱峰同时进行Full-MS实验。通过跟踪高度解析的低m / z来实现选择性峰选择含磷产物的产物离子，表示多个磷酸盐和膦酸酯基团。然后，通过同时精确地测量前体离子的质量以及已确证的可疑峰中存在的磷原子，来指定化学式。各种含磷化合物（例如V级化学战剂，神经毒剂的降解产物，农药，有机磷酸盐和磷脂）证明了这种新方法。对于这些化合物，发现开发的方法在土壤和尿液的环境提取物中（在磷脂的情况下）浓度低至1 ng / mL时都是有效的，使其可与选择性磷检测器（如GC- FPD，但对于带电荷，极性或更大的化合物具有更广泛的范围。