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

PeakstR (min)PolarityPrecursor IonProduct IonTransition TypePrecursorProductTransition Type
3.Methyl parathion7.75Positive263.0109.0Quantifier263.079.0Qualifier
ColumnRxi-5ms, 30 m, 0.25 mm ID, 0.25 µm (cat.# 13423)
Standard/SampleCalifornia 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:1:1 Acetonitrile:(1:1 hexane:acetone, 1% acetic acid)
Conc.:9 ng/mL Expected concentration range in extract of hemp initially spiked at 100 ng/g
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 Temp.:70 °C (hold 1 min) to 220 °C at 30 °C/min to 240 °C at 5 °C/min to 315 °C at 10 °C/min (hold 10 min)
Carrier GasHe, constant flow
Flow Rate:1.4 mL/min
Transfer Line Temp.:290 °C
Analyzer Type:Quadrupole
Source Temp.:330 °C
Electron Energy:70 eV
Tune Type:PFTBA
Ionization Mode:EI
InstrumentThermo Scientific TSQ 8000 Triple Quadrupole GC-MS
Sample PreparationPulverized hemp (1 g) was weighed in a 15 mL polypropylene tube. The sample was fortified with pesticides and mycotoxins at 100 ng/g. A mix of internal standards was added at 100 ng/g. 5 mL of acetonitrile acidified with 1% acetic acid was added to the sample, and this was followed by 5 min vortex extraction at 2500 rpm. 200 µL of water were added to a 6 mL hydrophilic lipophilic balanced (HLB) Resprep polymeric SPE cartridge (200 mg) (cat.# 28451). Then, 3 mL of hemp extract were transferred to the cartridge. Vacuum was applied to collect the cleaned extract. After collecting all the sample, the vacuum was stopped and 300 µL of methanol were added to help elute all the target analytes (vacuum was reapplied, and the rinsing solvent was collected with the rest of the extract). 1 mL of cleaned supernatant was transferred to a Q-sep QuEChERS dSPE tube containing magnesium sulfate and C18 (cat.# 26242). The sample was vortexed briefly and centrifuged for 5 min. Finally, the extract was diluted in a 1:1 ratio with a 1:1 hexane:acetone (1% acetic acid) solution, and 1 µL was injected into the GC-MS/MS system.