Simultaneous high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS-MS) analysis of cyanide and thiocyanate from swine plasma
作者： Raj K. Bhandari , Erica Manandhar , Robert P. Oda , Gary A. Rockwood , Brian A. Logue
DOI: 10.1007/S00216-013-7536-3
关键词:
摘要: An analytical procedure for the simultaneous determination of cyanide and thiocyanate in swine plasma was developed validated. Cyanide were simultaneously analyzed by high-performance liquid chromatography tandem mass spectrometry negative ionization mode after rapid simple sample preparation. Isotopically labeled internal standards, Na13C15N NaS13C15N, mixed with (spiked nonspiked), proteins precipitated acetone, samples centrifuged, supernatant removed dried. The dried reconstituted 10 mM ammonium formate. reacted naphthalene-2,3-dicarboxaldehyde taurine to form N-substituted 1-cyano[f]benzoisoindole, while chemically modified monobromobimane an SCN-bimane product. method produced dynamic ranges 0.1–50 0.2–50 μM thiocyanate, respectively, limits detection nM 50 thiocyanate. For quality control precision, as measured percent relative standard deviation, below 8 %, accuracy within ±10 % nominal concentration. Following validation, successfully detected from cyanide-exposed swine.
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