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|Peaks||tR (min)||Precursor Ion||Product Ion||Collision Energy (CE)|
|Column||Rxi-5ms, 30 m, 0.25 mm ID, 0.25 µm (cat.# 13423)|
|Standard/Sample||Organic 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)|
|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 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|
|Transfer Line Temp.:||290 °C|
|Source Temp.:||280 °C|
|Instrument||Thermo Scientific TSQ 8000 Triple Quadrupole GC-MS|
|Sample Preparation||Sample 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.
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