Analysis of Benzodiazepines
Applications | 2023 | ShimadzuInstrumentation
Determination of benzodiazepines is critical in pharmaceutical quality control and forensic analysis due to their therapeutic use and abuse potential. A robust GC-MS method ensures reliable identification and quantification of these compounds across various matrices.
This study presents an analytical protocol for the simultaneous separation and detection of seven common benzodiazepines—oxazepam, lorazepam, diazepam, flunitrazepam, prazepam, clonazepam and alprazolam—at 15 µg/mL in a butyl chloride extract. The goal is to achieve high resolution and reproducible results using capillary gas chromatography coupled with mass spectrometry.
The method employs a temperature gradient starting at 200 °C, ramped at 15 °C/min to 330 °C with a 3 min hold. Helium is used as the carrier gas in a constant linear velocity mode of 50 cm/s. A splitless injection of 1 µL is performed at 280 °C, with a solvent delay of 4 min. Electron ionization (EI) is used, and mass spectra are acquired over 50–350 m/z after tuning with perfluorotributylamine (PFTBA).
The optimized conditions yield baseline separation of all seven benzodiazepines within a 12-minute run time. Mass spectral data confirm compound identities with distinct fragmentation patterns. The method demonstrates excellent reproducibility and sensitivity suitable for routine screening.
Advancements may include coupling with tandem mass spectrometry for enhanced selectivity, shorter columns or fast GC techniques for reduced analysis time, and integration with automated sample preparation platforms.
The described GC-MS method provides a fast, sensitive and reproducible approach for the simultaneous analysis of multiple benzodiazepines. It is well suited for both regulatory compliance and forensic applications.
GC/MSD, GC/SQ, GC columns, Consumables
IndustriesClinical Research
ManufacturerShimadzu
Summary
Importance of Topic
Determination of benzodiazepines is critical in pharmaceutical quality control and forensic analysis due to their therapeutic use and abuse potential. A robust GC-MS method ensures reliable identification and quantification of these compounds across various matrices.
Objectives and Overview of the Study
This study presents an analytical protocol for the simultaneous separation and detection of seven common benzodiazepines—oxazepam, lorazepam, diazepam, flunitrazepam, prazepam, clonazepam and alprazolam—at 15 µg/mL in a butyl chloride extract. The goal is to achieve high resolution and reproducible results using capillary gas chromatography coupled with mass spectrometry.
Methodology
The method employs a temperature gradient starting at 200 °C, ramped at 15 °C/min to 330 °C with a 3 min hold. Helium is used as the carrier gas in a constant linear velocity mode of 50 cm/s. A splitless injection of 1 µL is performed at 280 °C, with a solvent delay of 4 min. Electron ionization (EI) is used, and mass spectra are acquired over 50–350 m/z after tuning with perfluorotributylamine (PFTBA).
Instrumentation Used
- Gas chromatograph–mass spectrometer: Shimadzu GCMS-QP2010
- Column: SH-I-5Sil MS, 30 m × 0.25 mm I.D., 0.25 µm film thickness
- Transfer line temperature: 280 °C
- Source temperature: 200 °C
Main Results and Discussion
The optimized conditions yield baseline separation of all seven benzodiazepines within a 12-minute run time. Mass spectral data confirm compound identities with distinct fragmentation patterns. The method demonstrates excellent reproducibility and sensitivity suitable for routine screening.
Benefits and Practical Applications
- High-throughput analysis in pharmaceutical quality control laboratories
- Reliable forensic screening for benzodiazepine abuse
- Reduced analysis time with clear chromatographic resolution
Future Trends and Opportunities
Advancements may include coupling with tandem mass spectrometry for enhanced selectivity, shorter columns or fast GC techniques for reduced analysis time, and integration with automated sample preparation platforms.
Conclusion
The described GC-MS method provides a fast, sensitive and reproducible approach for the simultaneous analysis of multiple benzodiazepines. It is well suited for both regulatory compliance and forensic applications.
Content was automatically generated from an orignal PDF document using AI and may contain inaccuracies.
Similar PDF
Analysis of EU PCB Congeners
2023|Shimadzu|Applications
ERAS-1000-0097 GCMS MS SH Series SH-I-XLB Analysis of EU PCB Congeners 97 Keywords: environment, dioxin 1. PCB 31 2. PCB 28 3. PCB 52 4. PCB 101 5. PCB 118 6. PCB 153 7. PCB 138 8. PCB 180 9.…
Key words
xlb, xlbcongeners, congenerspcb, pcbdichloromethane, dichloromethanegcms, gcmspurge, purgeseries, seriesscan, scanionization, ionizationcarrier, carrierrange, rangegas, gasmin, minflow, flowcolumn
Analysis of Endocrine disrupting chemicals
2023|Shimadzu|Applications
ERAS-1000-0486 GC-MS MS SH Series SH-I-1MS Analysis of Endocrine disrupting chemicals 486 1. Androsterone 2. Dehydroepiandrosterone (DHEA) 3. 17-α-Estradiol 4. Estrone 5. 17-β-Estradiol 6. Testosterone 7. derivatization by-product (100 μg/mL each) Instrument : GCMS Column Column temp. Inj. vol. Inj.…
Key words
disrupting, disruptingscan, scanendocrine, endocrinechemicals, chemicalsseries, seriesionization, ionizationcarrier, carrierdetector, detectormode, moderate, rateinstrument, instrumentrange, rangegas, gasflow, flowcolumn
Analysis of Electrolyte Solution in Lithium Ion Rechargeable Battery
2023|Shimadzu|Applications
ERAS-1000-0466 GCMS MS SH Series SH-200MS Analysis of Electrolyte Solution in Lithium Ion Rechargeable Battery 466 Keywords: Carbonate, Organic solvents and additives 1 2 4 1. Dimethyl carbonate 2. Ethyl methyl carbonate 3. Vinylene carbonate 4. Ethylene carbonate 3 Instrument…
Key words
rechargeable, rechargeablescan, scanelectrolyte, electrolytebattery, batterylithium, lithiumgcms, gcmsevent, eventsplit, splitseries, seriesratio, ratioionization, ionizationcarrier, carriermode, modesolution, solutioninstrument
Analysis of Genotoxic impurities
2023|Shimadzu|Applications
ERAS-1000-0491 GCMS MS SH Series SH-I-624Sil MS Analysis of Genotoxic impurities 491 Keywords: Pharmaceutical 1. 2-Chloropropane 2. Bromoethane 3. 1-Chloropropane 4. 2-Bromopropane 5. Butyl chloride 6. 1-Bromobutane (1 μg/mL in DMSO) Instrument : GCMS Column Column temp. Inj. vol. Liner…
Key words
gcms, gcmsgenotoxic, genotoxicscan, scanvelocity, velocitynotes, notesliner, linerdelay, delaypurge, purgeimpurities, impuritiesseries, serieslinear, linearionization, ionizationcarrier, carriersolvent, solventdetector