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Comparison of Incurred Fludioxonil in Various Parts of Orange on Rxi-5ms

PeakstR (min)Precursor IonProduct IonCollision Energy (CE)
1.Fludioxonil18.1624812730
image
GC_FS0570
ColumnRxi-5ms, 30 m, 0.25 mm ID, 0.25 µm (cat.# 13423)
SampleWhole orange QuEChERS extract (318 ng/g)
Orange peel QuEChERS extract (594 ng/g)
Orange pulp QuEChERS extract (6.8 ng/g)
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
NotesSample Preparation (adapted from EN and AOAC QuEChERS methods):

Orange (Whole): 10 g of homogenized orange was fortified with an internal standard and mixed with 10 mL acetonitrile and two steel ball bearings (1/16'') and shaken for 10 minutes. Q-sep QuEChERS extraction salts for EN 15662 (cat.# 25849) were added, and the sample was shaken for 1 minute. The sample was centrifuged for 5 minutes, and the supernatant was removed and further cleaned up with prefilled Q-sep QuEChERS dSPE tubes containing 150 mg MgSO4, 50 mg PSA, and 50 mg C18-EC (cat.# 26125).

Orange Peel: 10 g of homogenized orange peel was fortified with an internal standard, hydrated with 4 mL water, and briefly shaken by hand. Acetonitrile (10 mL) was added, and the sample was shaken for an additional 1 minute. Q-sep QuEChERS extraction salts for EN 15662 (cat.# 25849) were added, and the sample was shaken for 1 minute. The sample was centrifuged for 5 minutes, and the supernatant was removed and further cleaned up with prefilled Q-sep QuEChERS dSPE tubes containing 150 mg MgSO4, 25 mg PSA, and 25 mg C18-EC (cat.# 26216).

Orange Pulp: 15 g of homogenized orange pulp was fortified with an internal standard. Acetonitrile with 1% acetic acid (15 mL) was added, and the sample was shaken for 1 minute. Q-sep QuEChERS extraction salts for AOAC 2007.01 (cat.# 25851) were added, and the sample was shaken for an additional 1 minute. The sample was centrifuged for 5 minutes, and the supernatant was removed and further cleaned up with prefilled Q-sep QuEChERS dSPE tubes containing 150 mg MgSO4 and 50 mg PSA (cat.# 26124).

The dSPE supernatant of all samples was analyzed directly (no further dilution) within 24 hours of the initial extraction.
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