share:
delim
delim
GCxGC-TOFMS Analysis of Unfortified Tobacco Extract After QuEChERS Extraction and dSPE Cleanup With 25 mg PSA and 7.5 mg GCB

GCxGC-TOFMS Analysis of Unfortified Tobacco Extract After QuEChERS Extraction and dSPE Cleanup With 25 mg PSA and 7.5 mg GCB

image
GC_FF1242
ColumnRxi-5Sil MS 30 m, 0.25 mm ID, 0.25 µm (cat.# 13623)
Rtx-200 1.3 m, 0.25 mm ID, 0.25 µm (cat.# 15124)
SampleTobacco extract with dSPE cleanup
Injection
Inj. Vol.:1.0 µL splitless (hold 1.0 min)
Liner:Premium 4 mm single taper w/wool (cat.# 23303.5)
Inj. Temp.:250 °C
Oven
Oven Temp.:Rxi-5Sil MS: 90 °C (hold 1.0 min) to 310 °C at 5 °C/min (hold 2.0 min)
Rtx-200: 95 °C (hold 1.0 min) to 315 °C at 5 °C/min (hold 2.0 min)
Carrier GasHe, corrected constant flow (2 mL/min)
Modulation
Modulator Temp. Offset:+20 °C
Second Dimension Separation Time:3 sec
Hot Pulse Time:0.9 sec
Cool Time between Stages:0.6 sec
DetectorMS
Mode:
Transfer Line Temp.:300 °C
Analyzer Type:TOF
Source Temp.:225 °C
Electron Energy:70 eV
Mass Defect:-20 mu/100 u
Ionization Mode:EI
Acquisition Range:45 to 550 amu
Spectral Acquisition Rate:100 spectra/sec
InstrumentLECO Pegasus 4D GCxGC-TOFMS
NotesRtx-200 (cat.# 15124) is a 2 m column. A 1.3 m section was cut off and used as the second dimension column.

QuEChERS Extraction:
A 2 g sample of tobacco was weighed into a 50 mL polypropylene centrifuge tube (cat.# 26239). After the addition of 10 mL of organic-free water to the sample, 100 µL of QuEChERS internal standard mix for GC-MS analysis (cat.# 33267) was added to each sample. Next, 10 mL of acetonitrile was added and the samples were vortexed for 30 min. Immediately after vortexing, pre-packaged QuEChERS European EN 15662 method formulation extraction salts (cat.# 26236) were added to each centrifuge tube. The tubes were immediately shaken for 1 min and then centrifuged for 5 min at 3,000 g.

Sample Cleanup:
A 1 mL aliquot of the extract was fortified with 5 µL of an anthracene standard (cat.# 33264) and added to a dSPE tube containing 150 mg MgSO4, 25 mg PSA and 7.5 mg GCB (cat.# 26218). The tubes were gently shaken for 2 min and then centrifuged for 5 min using a Q-sep 3000 centrifuge (cat.# 26230). A 0.5 mL portion of the supernatant extract was removed and placed into an autosampler vial and 5 µL of a 5% formic acid solution in acetonitrile was added to each sample prior to analysis.
Download PDF

RELATED CHROMATOGRAM LIBRARY SEARCHES

pesticides

,

GCxGC

,

OCP

,

Organonitrogen

,

Organophosphorous

,

Organochlorine

,

Tobacco

Printing tips! To print chromatograms full page, change the print settings in the print dialogue window of your PDF reader software: 1) "fit" or "fit to page", 2) "landscape" for wide chromatograms or "portrait" for tall chromatograms.


Restek Domestic Customer Service

Subject

Message

Your Full Name

Your Email

Company Name

Address

Spam Block (Please leave this blank)

all fields required

Thank you

Your message has been sent. We will be in touch shortly.

Message not sent

Sorry, your message could not be sent at this time. Please try again later, or contact Restek or your local Restek representative via phone.

www.restek.com/Contact-Us