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Peaks | tR (min) | Precursor Ion | Product Ion | Collision Energy (CE) | |
---|---|---|---|---|---|
1. | Fludioxonil | 18.16 | 248 | 127 | 30 |
Column | Rxi-5ms, 30 m, 0.25 mm ID, 0.25 µm (cat.# 13423) |
---|---|
Standard/Sample | Whole 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 Gas | He, constant flow |
Flow Rate: | 1.4 mL/min |
Detector | TSQ 8000 |
---|---|
Transfer Line Temp.: | 290 °C |
Analyzer Type: | Quadrupole |
Source Temp.: | 280 °C |
Tune Type: | PFTBA |
Ionization Mode: | EI |
Instrument | Thermo Scientific TSQ 8000 Triple Quadrupole GC-MS |
Sample Preparation | Sample 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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