Simultaneous determination of flunitrazepam and 7-aminoflunitrazepam in human serum by ion trap gas chromatography-tandem mass spectrometry.

Simultaneous determination of flunitrazepam and 7-aminoflunitrazepam in human serum by ion trap gas chromatography-tandem mass spectrometry.

Legal medicine (Tokyo, Japan) (2003-08-26)

Masaru Terada, Sousuke Masui, Takeshi Hayashi, Ritsuko Watanabe, Hiromasa Inoue, Morio Iino, Masato Nakatome, Ryoji Matoba, Tatsuo Shinozuka, Tatsuya Murai, Einosuke Tanaka, Katsuya Honda

PMID12935562

ABSTRACT

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.

MATERIALS

Product Number

Brand

Product Description

A-911

Supelco

7-Aminoflunitrazepam solution, 1.0 mg/mL in acetonitrile, ampule of 1 mL, certified reference material, Cerilliant^®

A-912

Supelco

7-Aminoflunitrazepam solution, 100 μg/mL in acetonitrile, ampule of 1 mL, certified reference material, Cerilliant^®