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GC-Amenable Pesticides Regulated by California in Chocolate on Low-Pressure GC (LPGC) Column Kit

GC_GN1209
PeakstR (min)PolarityPrecursor IonProduct IonTransition Type
1.Atrazine-d54.57Positive220.058.0Quantifier
2.Atrazine-d54.57Positive205.0127.0Qualifier
3.Quintozene4.70Positive294.9236.9Quantifier
4.Quintozene4.70Positive236.8118.9Qualifier
5.Methyl parathion4.96Positive263.0109.0Quantifier
6.Methyl parathion4.96Positive263.079.0Qualifier
7.Captan5.47Positive184.0149.1Quantifier
8.Captan5.47Positive184.0134.1Qualifier
9.trans-Chlordane5.48Positive271.9237.0Quantifier
10.trans-Chlordane5.48Positive372.9265.9Qualifier
11.cis-Chlordane5.56Positive372.9265.9Quantifier
12.cis-Chlordane5.56Positive271.9237.0Qualifier
13.Chlorfenapyr5.69Positive247.1227.1Quantifier
14.Chlorfenapyr5.69Positive59.131.1Qualifier
15.Cyfluthrin6.71Positive226.0206.0Quantifier
16.Cyfluthrin6.71Positive163.0127.0Qualifier
17.Cypermethrin6.80Positive163.0127.1Quantifier
18.Cypermethrin6.80Positive181.1152.1Qualifier
ColumnLow-pressure GC column kit (factory-coupled restrictor column [5 m x 0.18 mm ID] and Rtx-5ms analytical column [15 m, 0.53 mm ID, 1 µm plus 1 m integrated transfer line on the outlet end]) (cat.# 11800)
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:Acetonitrile
Conc.:5.8-8.4 ng/mL Expected concentration range (70-100% recovery) in extract after extracting from chocolate fortified at 100 ng/g (final extract was diluted in half with acidified 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.:80 °C (hold 1 min) to 330 °C at 45 °C/min (hold 5.5 min)
Carrier GasHe, constant flow
Flow Rate:2.0 mL/min
DetectorMS/MS
Transfer Line Temp.:290 °C
Analyzer Type:Quadrupole
Source Temp.:325 °C
Electron Energy:70 eV
Tune Type:PFTBA
Ionization Mode:EI
InstrumentThermo Scientific TSQ 8000 Triple Quadrupole GC-MS
NotesChocolate was pulverized using a SPEX Freezer/Mill grinder, and 0.5 g sample was fortified with pesticides and mycotoxins at 100 ng/g. A mix of internal standards was added at 200 ng/g. Then, 0.5 mL of isopropyl alcohol was added to the sample. The sample was vortexed for 10 sec or until a homogenous mixture was obtained. Afterwards, 2.5 mL of acetonitrile acidified with acetic acid at 1% v/v was added to the vial. Once again, the mixture was vortexed for 30 sec, and then centrifuged for 5 min at 4300 ×g at room temperature. A total of 2 mL of the supernatant was passed through 100 mg Resprep C18 SPE cartridge (cat.# 26030). 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.