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GC Amenable Pesticides Regulated by California in Brownies on Rxi-5ms

Column | Rxi-5ms, 30 m, 0.25 mm ID, 0.25 µm (cat.# 13423) |
Sample | California pesticide standard #1 (cat.# 34124) |
California pesticide standard #2 (cat.# 34125) | |
California pesticide standard #3 (cat.# 34126) | |
California pesticide standard #4 (cat.# 34127) | |
California pesticide standard #5 (cat.# 34128) | |
California pesticide standard #6 (cat.# 34129) | |
Atrazine-d5 (cat.# 31984) | |
Diluent: | Acetonitrile |
Conc.: | 5-7.5 ng/mL Expected concentration range in extract after extracting from brownie fortified at 100 ng/g (final extract was diluted in half with acetonitrile). |
Injection | |
Inj. Vol.: | 1 µL splitless |
Liner: | Topaz 4.0 mm ID single taper inlet liner w/wool (cat.# 23447) |
Inj. Temp.: | 250 °C |
Purge Flow: | 5 mL/min |
Oven | |
Oven Temp.: | 90 °C (hold 1 min) to 310 °C at 25 °C/min (hold 10 min) |
Carrier Gas | He, constant flow |
Flow Rate: | 1.4 mL/min |
Detector | MS/MS |
Transfer Line Temp.: | 290 °C |
Analyzer Type: | Quadrupole |
Source Temp.: | 330 °C |
Electron Energy: | 70 eV |
Tune Type: | PFTBA |
Ionization Mode: | EI |
Instrument | Thermo Scientific TSQ 8000 Triple Quadrupole GC-MS |
Notes | Brownies were pulverized using a SPEX Freezer/Mill grinder and 0.5 g samples were fortified with pesticides and mycotoxins at 100 ng/g. A mix of internal standards was added at 200 ng/g. 1.5 mL of acetonitrile acidified with 1% acetic acid was added to the sample. The sample was vortexed and sonicated for 5 min, then the supernatant was passed through a 100 mg Resprep SPE C18 cartridge (cat.# 26030). An additional 1.5 mL of extraction solvent (acidified acetonitrile) was added to the sample pellet, and the sample was vortexed again. The supernatant was passed through the same C18 cartridge. After reserving 750 μL for LC-MS analysis, the remaining supernatant was transferred to a Q-sep QuEChERS dSPE tube containing pre-weighed magnesium sulfate and PSA (cat.# 26215). After vortexing and centrifuging, 500 μL of extract was mixed with 500 μL of acidified acetonitrile. 1 μL of final extract was injected into the GC-MS/MS system. |
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