Innovative Chromatography Products
www.restek.it
www.restek.it
Questo cromatogramma potrebbe contenere analiti che sono sinonimi dei vostri parametri di ricerca.
GCxGC-TOFMS Analysis of Unfortified Tobacco Extract After QuEChERS Extraction and dSPE Cleanup With 25 mg PSA and 7.5 mg GCB
GC_FF1242
| Column | Rxi-5Sil MS 30 m, 0.25 mm ID, 0.25 µm (cat.# 13623) |
| Rtx-200 1.3 m, 0.25 mm ID, 0.25 µm (cat.# 15124) | |
| Sample | Tobacco extract with dSPE cleanup |
| Injection | |
| Inj. Vol.: | 1.0 µL splitless (hold 1.0 min) |
| Liner: | Premium 4 mm single taper w/wool (cat.# 23303.5) |
| Inj. Temp.: | 250 °C |
| Oven | |
| Oven Temp.: | Rxi-5Sil MS: 90 °C (hold 1.0 min) to 310 °C at 5 °C/min (hold 2.0 min) Rtx-200: 95 °C (hold 1.0 min) to 315 °C at 5 °C/min (hold 2.0 min) |
| Carrier Gas | He, corrected constant flow (2 mL/min) |
| Modulation | |
| Modulator Temp. Offset: | +20 °C |
| Second Dimension Separation Time: | 3 sec |
| Hot Pulse Time: | 0.9 sec |
| Cool Time between Stages: | 0.6 sec |
| Detector | MS |
| Mode: | |
| Transfer Line Temp.: | 300 °C |
| Analyzer Type: | TOF |
| Source Temp.: | 225 °C |
| Electron Energy: | 70 eV |
| Mass Defect: | -20 mu/100 u |
| Ionization Mode: | EI |
| Acquisition Range: | 45 to 550 amu |
| Spectral Acquisition Rate: | 100 spectra/sec |
| Instrument | LECO Pegasus 4D GCxGC-TOFMS |
| Notes | Rtx-200 (cat.# 15124) is a 2 m column. A 1.3 m section was cut off and used as the second dimension column. QuEChERS Extraction: A 2 g sample of tobacco was weighed into a 50 mL polypropylene centrifuge tube (cat.# 26239). After the addition of 10 mL of organic-free water to the sample, 100 µL of QuEChERS internal standard mix for GC-MS analysis (cat.# 33267) was added to each sample. Next, 10 mL of acetonitrile was added and the samples were vortexed for 30 min. Immediately after vortexing, pre-packaged QuEChERS European EN 15662 method formulation extraction salts (cat.# 26236) were added to each centrifuge tube. The tubes were immediately shaken for 1 min and then centrifuged for 5 min at 3,000 g. Sample Cleanup: A 1 mL aliquot of the extract was fortified with 5 µL of an anthracene standard (cat.# 33264) and added to a dSPE tube containing 150 mg MgSO4, 25 mg PSA and 7.5 mg GCB (cat.# 26218). The tubes were gently shaken for 2 min and then centrifuged for 5 min using a Q-sep 3000 centrifuge (cat.# 26230). A 0.5 mL portion of the supernatant extract was removed and placed into an autosampler vial and 5 µL of a 5% formic acid solution in acetonitrile was added to each sample prior to analysis. |
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