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

GC_GN1207
PeakstR (min)PolarityPrecursor IonProduct IonTransition Type
1.Atrazine-d56.82Positive220.058.0Quantifier
2.Atrazine-d56.82Positive205.0127.0Qualifier
3.Diazinon-d10 (diethyl-d10)7.01Positive183.0139.0Quantifier
4.Diazinon-d10 (diethyl-d10)7.01Positive183.0168.0Qualifier
5.Quintozene7.03Positive294.9236.9Quantifier
6.Quintozene7.03Positive236.8118.9Qualifier
7.Methyl parathion7.50Positive263.0109.0Quantifier
8.Methyl parathion7.50Positive263.079.0Qualifier
9.Captan8.37Positive184.0149.1Quantifier
10.Captan8.37Positive184.0134.1Qualifier
11.trans-Chlordane8.41Positive271.9237.0Quantifier
12.trans-Chlordane8.41Positive372.9265.9Qualifier
13.cis-Chlordane8.53Positive372.9265.9Quantifier
14.cis-Chlordane8.53Positive271.9237.0Qualifier
15.Chlorfenapyr8.80Positive247.1227.1Quantifier
16.Chlorfenapyr8.80Positive59.131.1Qualifier
17.Cyfluthrin10.61Positive226.0206.0Quantifier
18.Cyfluthrin10.61Positive163.0127.0Qualifier
19.Cypermethrin10.87Positive163.0127.1Quantifier
20.Cypermethrin10.87Positive181.1152.1Qualifier
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)
Diazinon-d10 (cat.# 31986)
Diluent:Acetonitrile
Conc.:2.5-10 ng/mL Expected concentration range in extract after extracting from gummy 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
NotesGummies were manually chopped into small pieces, and 1 g of sample was weighed in a 50 mL polypropylene tube. The sample was mixed with 5 mL of water and then vigorously vortexed until all gummy pieces were fully solubilized. The sample was fortified with pesticides and mycotoxins at 100 ng/g. A mix of internal standards was added at 200 ng/g. The spiked sample was further vortexed for 30 sec. 5 mL of acetonitrile acidified with 1% acetic acid was added to the sample, and this was followed by 30 sec vortex agitation. Then, a pouch of European EN 15662 QuEChERS extraction salts (cat.# 25849) was added to the sample. The sample was vortexed for 30 sec and then centrifuged for 5 min. 1.9 mL of supernatant was transferred to a Q-sep QuEChERS dSPE tube containing pre-weighed magnesium sulfate, PSA, and GCB (cat.# 26217). 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.