Application of selected reaction monitoring tandem mass spectrometry to the quantitative determination of an arsenic-containing nucleoside in a crude biological extract

Analyst

Volumn 129, Issue 5, 2004, Pages 398-399

  Francesconi, Kevin A ^a   Pergantis, Spiros A ^b  

^a UNIVERSITY OF GRAZ   (Austria)

^b UNIVERSITY OF CRETE   (Greece)

Author keywords

[No Author keywords available]

Indexed keywords

5' DIMETHYLARSINOYLADENOSINE; ARSENIC; NUCLEOSIDE; UNCLASSIFIED DRUG;

ACCURACY; ARTICLE; BIOLOGICAL MONITORING; CLAM; CONTROLLED STUDY; EXTRACT; HIGH PERFORMANCE LIQUID CHROMATOGRAPHY; KIDNEY; NONHUMAN; QUANTITATIVE ANALYSIS; REACTION ANALYSIS; TANDEM MASS SPECTROMETRY; TRIDACNA DERASA;

EID: 2442658951     PISSN: 00032654     EISSN: None     Source Type: Journal    
DOI: 10.1039/b402876g     Document Type: Article

References (12)

1. J. Szpunar, Analyst, 2000, 963.
2. K. A. Francesconi and J. S. Edmonds, Rapid Commun. Mass Spectrom., 2001, 15, 1641.
3. S. McSheehy, J. Szpunar, R. Lobinski, V. Haldys, J. Tortajada and J. S. Edmonds, Anal. Chem., 2002, 74, 2370.
4. K. A. Francesconi, J. S. Edmonds and R. V. Stick, J. Chem. Soc., Perkin Trans. I, 1992, 1349.
5. -1.
6. An electrospray triple quadrupole mass spectrometer (TSQ Quantum, Thermo Electron) in combination with a HPLC pump and an autosampler (Surveyor, Thermo Electron) was used throughout this study.
7. The CID breakdown curves are available as electronic supplementary material.†.
8. -1; the effluent was split post-column with 16% being directed to the ES MS. Injection volumes were 20 μl.
9. Limit of detection was determined with mobile phase containing 3% methanol, and defined as the analyte concentration giving a signal equal to the blank plus three standard deviations of the blank. The HPLC window of 3.5-6.0 min was used to measure blank signals for 7 consecutive runs.
10. 2,3 Extracts were prepared by weighing a portion (17.8 mg) of the fine powder into an Eppendorf tube, adding 1.00 mL of 20 mM ammonium bicarbonate, pH 10.0 (HPLC stock mobile phase), and shaking for about two min. The mixture was centrifuged (13,000 rpm, 5 min) and the clear, brown supernatant was analysed directly or after diluting with mobile phase (1 + 1).
11. -1 of standard 5′- dimethylarsinoyladenosine.
12. A minimum value based on complete extraction of the target compound. We have not optimised the extraction procedure, but our previous experience with water-soluble arsenicals indicates high extraction efficiency with this simple procedure.