离子阱气相色谱-串联质谱法同时测定人血清中氟硝西泮和7-氨基氟硝西泮
Simultaneous determination of flunitrazepam and 7-aminoflunitrazepam in human serum by ion trap gas chromatography-tandem mass spectrometry.
作者信息
Terada Masaru, Masui Sousuke, Hayashi Takeshi, Watanabe Ritsuko, Inoue Hiromasa, Iino Morio, Nakatome Masato, Matoba Ryoji, Shinozuka Tatsuo, Murai Tatsuya, Tanaka Einosuke, Honda Katsuya
机构信息
Course of Social Medicine, Department of Legal Medicine, Osaka University Graduate School of Medicine F3, Suita-shi, Osaka 565-0871, Japan.
出版信息
Leg Med (Tokyo). 2003 Mar;5 Suppl 1:S96-S100. doi: 10.1016/s1344-6223(02)00075-5.
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.
建立了一种采用离子阱气相色谱（GC）-串联质谱法测定人血清中氟硝西泮（FNZ）和7-氨基氟硝西泮（7-AFNZ）的方法。7-AFNZ用50微升三氟乙酸酐（TFAA）在60℃下衍生20分钟。FNZ和7-AFNZ-TFA的EI质谱和串联质谱分别为m/z 238、239、266、286、294、312、313（M(+)），m/z 350、351、360、378、379（M(+)），m/z 238、239、240（母离子m/z 286，碰撞能量1.5 V），以及m/z 239、254、264、336（母离子m/z 351，碰撞能量1.8 V）。人血清中FNZ和7-AFNZ的全扫描EI质谱和串联质谱的检测限分别约为200 ng/ml、60 ng/ml、15 ng/ml和1 ng/ml。
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