001_TOC.qxp - page 143

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GCCHROMATOGRAMS |
PHARMACEUTICAL
Pesticides in Dietary Supplements
dSPEvs. cSPESampleCleanupofDandelionRootPowder (DietarySupplement)
Rxi®-5SilMS
GC_FF1171
Column
Rxi
®
-5Sil MS, 30m, 0.25mm ID, 0.25µm (cat.# 13623)
Sample
Dandelion Root powder spikedwith 46 pesticides
QuEChERS Internal StandardMix for GC/MS Analysis (cat.# 33267)
anthracene for quality control (cat.# 33264)
Conc.:
80 pg/µL
Injection
Inj. Vol.:
1µL splitless (hold 1.5min.)
Liner:
5mm Splitlesswithwool (cat.# 22975-200.1)
Inj.Temp.:
250 °C
Oven
OvenTemp:
90 °C (hold 1.5min.) to 340 °C at 8 °C/min.
Carrier Gas
He, constant flow
FlowRate:
1.5mL/min.
Detector
MS
Mode:
AnalyzerType:
TOF
SourceTemp.:
225 °C
Electron Energy:
70 eV
IonizationMode:
EI
Acquisition Range: 45-550 amu
Acquisition Rate:
5 spectra/sec.
Instrument
LECO Pegasus 4DGCxGC-TOFMS
Notes
Sample Preparation:
Wetting: 1 g of Dandelion Root powder combinedwith 9mL of water, shakenwell, fortifiedwith pesticides andQuEChERS Internal Standard
Mix for GC/MS Analysis (cat.# 33267), soak for 2 hours.
Extraction: 10mL acetonitrile added then addition of Q-sep™Q110 (cat.# 26235), centrifugewithQ-sep™ 3000 Centrifuge (cat.# 26230).
dSPE: cleanup procedure according to EN 15662method, add control standard anthracene (cat.# 33264) to 1mL extract, add this toQ-sep™
Q110 dSPE tube (cat.# 26235), shake, centrifuge.
cSPE: add control standard anthracene (cat.# 33264) to 1mL extract, addmagnesium sulfate to cartridge, use 6mL Combo SPE Cartridge
containing 500mg CarboPrep
®
90/500mg PSA (cat.# 26194), concentrate via evaporation.
NEW!
free
literature
DevelopingNewMethodsforPesticides inDietarySupplements
Advantagesof theQuEChERSApproach
QuEChERS isasimple, effectiveapproach tosampleprep thatcanbeapplied to theanalysis
ofpesticides indietarysupplements.HerewedemonstrateaQuEChERS, cSPE,GC-TOFMS
procedure that results ingood recoveries forawide rangeofpesticides indandelion root.
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ApplicationsNote
lit.cat.#PHAN1242
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TelNo : 03 9762 2034 . . . inAUSTRALIA
Mar 2011
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