Evaluation of an improved general unknown screening procedure using liquid chromatography-electrospray-mass spectrometry by comparison with gas chromatography and high-performance liquid-chromatography--diode array detection.

摘要: This paper presents an improved, comprehensive liquid chromatography-electrospray-mass spectrometry (LC-ES-MS) general unknown screening (GUS) procedure for drugs and toxic compounds its comparison with conventional techniques in routine laboratory conditions. Chromatographic separation involved X-TERRA MS C18, 3.5 µm (100 mm × 1 i.d.) column together a 25-min long gradient of acetonitrile pH 3, 2 mM ammonium formate delivered at 50 µl/min flow rate. Two different in-source collision-induced dissociation voltages were alternated, both the positive negative ion modes. Reconstructed spectra then obtained polarities by adding up low high energy, resulting presenting sufficient number specific fragment ions unambiguous fast identification compounds. large mass spectral libraries built efficient automated signal processing, library searching report editing algorithm developed. Using common, solid-phase extraction procedure, this LC-ES-MS technique was compared to GC-MS HPLC-DAD GUS procedures priori 51 serum samples consecutively sent GUS. The present LC-MS method identified 75% contained these (versus 66% 71% HPLC-DAD), including 8% that other two failed identify 9.5% HPLC-DAD). Therefore, it is complementary and/or helps enlarge range detected clinical toxicology. It could be useful as well forensic toxicology confirm result, 38% all three 36% them.