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

PeakstR (min)PolarityPrecursor IonProduct IonTransition Type
1.Atrazine-D57.5Positive220.058.0Quantifier
2.Atrazine-D57.5Positive205.0127.0Qualifier
3.Quintozene7.8Positive294.9236.9Quantifier
4.Quintozene7.8Positive236.8118.9Qualifier
5.Methyl parathion8.2Positive263.0109.0Quantifier
6.Methyl parathion8.2Positive263.079.0Qualifier
7.Captan9.1Positive184.0149.1Quantifier
8.Captan9.1Positive184.0134.1Qualifier
9.trans-Chlordane9.1Positive271.9237.0Quantifier
10.trans-Chlordane9.1Positive372.9265.9Qualifier
11.cis-Chlordane9.3Positive372.9265.9Quantifier
12.cis-Chlordane9.3Positive271.9237.0Qualifier
13.Chlorfenapyr9.5Positive247.1227.1Quantifier
14.Chlorfenapyr9.5Positive59.131.1Qualifier
15.Cyfluthrin11.5Positive163.0127.1Quantifier
16.Cyfluthrin11.5Positive199.1170.1Qualifier
17.Cypermethrin11.7Positive163.0127.1Quantifier
18.Cypermethrin11.7Positive181.1152.1Qualifier
image
GC_GN1206
ColumnRxi-5ms, 30 m, 0.25 mm ID, 0.25 µm (cat.# 13423)
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: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 GasHe, constant flow
Flow Rate:1.4 mL/min
DetectorMS/MS
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
NotesBrownies 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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