Preparation of Mass spectrum library of various medicines for LC/MS measurement

• Project/Area Number: 15591923
• Research Category: Grant-in-Aid for Scientific Research (C)
• Allocation Type: Single-year Grants
• Section: 一般
• Research Field: Emergency medicine
• Research Institution: Aichi Medical University School of Medicine
• Principal Investigator: HATTORI Hideki Aichi Medical University, School of Medicine, Associate Professor, 医学部, 助教授 (30107817)
• Project Period (FY): 2003 – 2004
• Project Status: Completed (Fiscal Year 2004)
• Budget Amount: ¥3,600,000 (Direct Cost: ¥3,600,000); Fiscal Year 2004: ¥1,000,000 (Direct Cost: ¥1,000,000); Fiscal Year 2003: ¥2,600,000 (Direct Cost: ¥2,600,000)
• Keywords: library / Iontrap type LC / MS / LCQ / MS spectrum / Positive / ESI mode / Xcalibur / LC / ESIポジティブイオン / イオンストラップ / 薬物

Research Abstract

We have constructed MS and MS/MS spectrum libraries of about 200 drugs using an LCQ LC/MS system. In most drugs, MS and MS/MS spectra were obtained. Barbiturates and organophosphorus pesticides were not fully ionized and impossible to obtain spectra. The LC conditions were : The elution gradient was 0 % B (100 % A 5 min hold) to 80 % B (20 % A) over 20 min at flow rate of 0.2 ml/min:solvent A was distilled water containing 7.5 mM ammonium acetate, and solvent B acetonitrile containing 0.05 % formic acid. The MS conditions were ionization, positive ESI ; capillary temperature, 270゜C ; Sheath gas flow and auxiliary gas flow, 90 and 30 unit (arbitrary unit) ; source voltage, 5.80 kV ; capillary voltage, 16V ; max ion time, 200ms ; respectively. The M /MS conditions were : isolation width, 2.0 m/z; normalized collision energy, 40 %, respectively. Using the column enable direct injection of crude sample, most compounds seemed to be sufficiently separated Our results suggest the above conditions are useful and applicable for the screening of drugs in clinical and forensic toxicology.