LAAN-E-MS-E028 GCMS Gas Chromatograph Mass Spectrometer Analysis of a Benzodiazepine-Based Drug Using GC-MS 28 Benzodiazepine drugs are commonly used in sleeping aids and tranquilizers, and sometimes in crimes or suicide. Therefore, these chemical substances are often analyzed by forensic laboratories for criminal or academic investigations. This datasheet shows the results from using GC-MS to measure 9 types of benzodiazepine drugs. Analysis Conditions Table 1: Analysis Conditions GC-MS :GCMS-QP2010 Ultra Column : Rxi®-5Sil MS （30 mL. X 0.25 mmI.D., df=0.25 µm, Shimadzu GLC P/N:13623) Glass insert :Silanized splitless insert (P/N: 221-48876-03) [GC] [MS] Vaporization chamber temperature : 260℃ Interface temperature : 280℃ Column oven temperature : 60℃ (2min) -> (10℃/min) -> 320℃ (10min) Ion source temperature : 200℃ Injection mode : Splitless Solvent elution time : 2.0 min Sampling time : 1 min Measurement mode : Scan High pressure injection method: 250 kPa (1.5 min) Mass range : m/z 35-600 Carrier gas : Helium Event time : 0.3 sec Control mode :Linear velocity (45.6 cm/sec) Emission current : 150 µA (high sensitivity) Purge flow rate :3.0 ml/min Sample injection quantity :1.0 µL (x1,000,000) 3.0 3 2.5 2 2.0 1.5 1.0 1 0.5 22.0 23.0 24.0 25.0 26.0 27.0 28.0 min % % 312 55 100.0 1 285 100.0 2 313 109 75.0 75.0 266 259287 342 166 50.0 238 50.0 248 25.0 183 25.0 63 109 0.0 0.0 100 200 300 400 100 200 300 400 % 86 100.0 3 75.0 50.0 25.0 58 99 183 315 387 0.0 100 200 300 400 Fig. 1: Total Ion Current Chromatogram and Mass Spectra 1: Flunitrazepam, 2: Flutoprazepam, 3: Flurazepam 28 (x1,000,000) TIC 3.5 5 3.0 2.5 4 7 2.0 1.5 6 1.0 0.5 17.5 20.0 22.5 25.0 27.5 30.0 min % % 45256 274 100 100 302 283 50 50 221 285 239 283 109 183 110 165 75 211 51 193 241 0 0 100 200 300 100 200 300 % % 67259 342 100 100 205 294 50 50 77 239 313 51 102 137 224 266 163 137 0 0 100 200 300 100 200 300 Fig. 2: Total Ion Current Chromatogram and Mass Spectra 4: Fludiazepam, 5: Diazepam, 6: Estazolam, 7: Etizolam (x1,000,000) 2.0 TIC 8 9 1.5 1.0 0.5 19.0 20.0 21.0 22.0 23.0 24.0 25.0 26.0 min % % 8 207 9 310 100 242 100 50 50 325 165 270 227 128 163 222 297 0 0 100 200 300 100 200 300 Fig. 3: Total Ion Current Chromatogram and Mass Spectra 8: Medazepam, 9: Midazolam For Research Use Only. Not for use in diagnostic procedures. Shimadzu Corporation (“Shimadzu”) reserves all rights including copyright in this publication. Shimadzu does not assume any responsibility or liability for any damage, whether direct or indirect, relating to, or arising out of the use of this publication. This publication is based upon the information available to Shimadzu on or before the date of publication, and subject to change without notice. First Edition: October 2011.