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Incurred 3,4-Dichloroaniline and N-(2,4-Dimethylphenyl)formamide in Honey on Rxi-5ms

GC_FS0575
PeakstR (min)Precursor IonProduct IonCollision Energy (CE)
1.3,4-Dichloraniline8.951619921
2.N-(2,4-Dimethylphenyl)formamide9.631207715
ColumnRxi-5ms, 30 m, 0.25 mm ID, 0.25 µm (cat.# 13423)
Standard/SampleOrganic honey QuEChERS extract (blank)
Honey QuEChERS extract (2.5 ppb and 8.9 ppb, respectively)
Organic honey QuEChERS extract (10 ppb each)
Organic honey QuEChERS extract (40 ppb each)
GC multiresidue pesticide kit (cat.# 32562)
Triphenylphosphate (IS) (cat.# 33258)
Diluent:Acetonitrile
Injection
Inj. Vol.:1 µL splitless (hold 0.5 min)
Liner:Topaz 4.0 mm ID single taper inlet liner w/wool (cat.# 23447)
Inj. Temp.:250 °C
Oven
Oven Temp.:90 °C (hold 1 min) to 330 °C at 8.5 °C/min (hold 5 min)
Carrier GasHe, constant flow
Flow Rate:1.4 mL/min
DetectorTSQ 8000
Transfer Line Temp.:290 °C
Analyzer Type:Quadrupole
Source Temp.:280 °C
Tune Type:PFTBA
Ionization Mode:EI
InstrumentThermo Scientific TSQ 8000 Triple Quadrupole GC-MS
Sample PreparationSample Preparation (Adapted AOAC QuEChERS Methods)
Organic Honey Calibration: 7.5 g of organic honey was spiked with an internal standard and the GC multiresidue pesticide mix at 100 ppb and hydrated with 15 mL water. The sample was shaken for 30 minutes. Acetonitrile with 1% acetic acid (15 mL) was added, and the sample was shaken for 1 minute. AOAC salts (cat.#25851) were added, and the sample was shaken for an additional minute. The sample was centrifuged for 5 minutes, and the supernatant was removed and further cleaned with Q-sep QuEChERS dSPE (cat.# 26124). This standard was further diluted with blank extract to 10 and 40 ppb and analyzed within 24 hours

Regular Honey and Organic Honey Blank: 7.5 g of honey was spiked with an internal standard and hydrated with 15 mL water. The samples were shaken for 30 minutes. Acetonitrile with 1% acetic acid (15 mL) was added, and the sample was shaken for 1 minute. AOAC salts (cat.# 25851) were added, and the samples were shaken for an additional minute. The samples were centrifuged for 5 minutes, and then the supernatant was removed and further cleaned with Q-sep QuEChERS dSPE (cat.# 26124). The samples were analyzed directly as dSPE supernatant within 24 hours of the initial extraction.