Simultaneous determination of flunitrazepam and 7-aminoflunitrazepam in human serum by ion trap gas chromatography-tandem mass spectrometry.
A method for the determination of flunitrazepam (FNZ) and 7-aminoflunitrazepam (7-AFNZ) in human serum was developed with ion trap gas chromatography (GC)-tandem mass spectrometry. The 7-AFNZ was derivatizated with 50 microl trifluoroacetic anhydride (TFAA), 60 degrees C-20 min. EI mass spectra and tandem mass spectra of FNZ and 7-AFNZ-TFA were m/z 238, 239, 266, 286, 294, 312, 313(M(+)), m/z 350, 351, 360, 378, 379(M(+)), m/z 238, 239, 240 (precursor ion m/z 286, collision energy 1.5 V), and m/z 239, 254, 264, 336 (precursor ion m/z 351, collision energy 1.8 V), respectively. The detection limits of full scan EI mass spectrometry and tandem mass spectrometry for FNZ and 7-AFNZ in human serum were ca. 200 ng/ml, 60 ng/ml, 15 ng/ml and 1 ng/ml, respectively.
Terada
Masaru
M
Course of Social Medicine, Department of Legal Medicine, Osaka University Graduate School of Medicine F3, Suita-shi, Osaka 565-0871, Japan. terada@legal.med.osaka-u.ac.jp
Masui
Sousuke
S
Hayashi
Takeshi
T
Watanabe
Ritsuko
R
Inoue
Hiromasa
H
Iino
Morio
M
Nakatome
Masato
M
Matoba
Ryoji
R
Shinozuka
Tatsuo
T
Murai
Tatsuya
T
Tanaka
Einosuke
E
Honda
Katsuya
K
D014151:Anti-Anxiety Agents / Q000097:blood* / Q000737:chemistry; D005445:Flunitrazepam / Q000031:analogs & derivatives* / Q000097:blood* / Q000737:chemistry; D005554:Forensic Medicine / Q000379:methods; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D015394:Molecular Structure; D012680:Sensitivity and Specificity
D014151:Anti-Anxiety Agents; D005445:Flunitrazepam; C036343:7-aminoflunitrazepam