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Column | Rxi-5Sil MS 30 m, 0.25 mm ID, 0.25 µm (cat.# 13623) |
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Rtx-200 1.5 m, 0.18 mm ID, 0.20 µm (cat.# 45001) | |
Standard/Sample | Pesticides in red bell pepper extract |
QuEChERS internal standard mix for GC-MS analysis (cat.# 33267) | |
Diluent: | Acetonitrile |
Injection | |
Inj. Vol.: | 1 µL splitless (hold 1 min) |
Liner: | Gooseneck splitless (5 mm) w/deactivated wool (cat.# 22973-200.1) |
Inj. Temp.: | 250 °C |
Purge Flow: | 40 mL/min |
Oven | |
Oven Temp.: | Rxi-5Sil MS: 90 °C (hold 1 min) to 310 °C at 4 °C/min (hold 2 min) Rtx-200: 100 °C (hold 1 min) to 320 °C at 4 °C/min (hold 2 min) |
Carrier Gas | He, corrected constant flow (1.8 mL/min) |
Modulation | |
Modulator Temp. Offset: | 25 °C |
Second Dimension Separation Time: | 4 sec |
Hot Pulse Time: | 1.2 sec |
Cool Time between Stages: | 0.8 sec |
Detector | TOFMS |
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Transfer Line Temp.: | 290 °C |
Analyzer Type: | TOF |
Source Temp.: | 225 °C |
Electron Energy: | 70 eV |
Mass Defect: | -20 mu/100 u |
Solvent Delay Time: | 5 min |
Tune Type: | PFTBA |
Ionization Mode: | EI |
Acquisition Range: | 45-550 amu |
Spectral Acquisition Rate: | 100 spectra/sec |
Instrument | LECO Pegasus 4D GCxGC-TOFMS |
Sample Preparation | Internal Standard: 100 µL of QuEChERS internal standard mix for GC-MS analysis (cat.# 33267) and 100 µL of QuEChERS internal standard mix for LC-MS/MS analysis (cat.# 33261) were added to each 10 g sample. These internal standard mixes require no dilutions and contain compounds specified in the EN 15662 QuEChERS method. Extraction: 10 mL acetonitrile was added to a 10 gram sample of homogenized red bell pepper. After a 1 minute shake, Q-sep European method extraction salts (cat.# 26236) were added followed by another 1 minute shake. The sample was then centrifuged with a Q-sep 3000 centrifuge (cat.# 26230). dSPE: Add 1 mL extract to QuEChERS dSPE cleanup tube containing 150 mg MgSO4, 25 mg PSA, and 25 mg C18 (cat.# 26216). Shake for 30 seconds and centrifuge with a Q-sep 3000 centrifuge (cat.# 26230). |
Notes | Rtx-200 (cat.# 45001) is a 10 m column. A 1.5 m section was cut off and used as the second dimension column. |
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