GC/MS/MS Analysis of Pesticides in Chamomile on SLB(R)-5ms after QuEChERS Cleanup usingSupelClean(TM) Ultra

GC/MS/MS Analysis of Pesticides in Chamomile on SLB®-5ms after QuEChERS Cleanup usingSupelClean™ Ultra

Conditions

sample/matrix chamomile
extraction tube Supel Que non-buffered extraction tube (4 mg NaSO4, 1 g NaCl in 12 mL tube) (55294-U)
extraction process Add 10 mL acetonitrile/IS Extraction Solvent and allow to sit 15 minutes, then shake or vortex 30 sec. Add contents of Supel Que non-buffered extraction tube (55294-U). (Shake by hand immediately to prevent clumping. Shake on shaker for 30 minutes at 2250 rpm, centrifuge for 5 minutes at 4500 rpm. Draw off supernatant for cleanup.)
clean-up process See description text
clean-up tube Supelclean Ultra 2400, 3 mL (54281-U)
column SLB-5ms, 30 m x 0.25 mm I.D. x 0.25 μm (28471-U)
oven 105°C (3 min), 10 °C/min to 130 °C, 4°C/min to 200°C, 8°C/min. to 300°C (10 min)
carrier gas helium, 1.4 mL/min constant flow
sample QuEChERS extract of chamomile
injection 2 μL splitless
liner 2 mm ID
inj. temp. programmed: 100 °C (.05 min), to 280 °C at 720°C/min, hold 45 min
detector MS/MS
MSD interface 300 °C
scan range MRM

Description

Analysis Note QuEChERS is a common method used for extraction of pesticide residues from dry botanicals. The resulting extracts are often very high in background, requiring a rigorous cleanup prior to analysis. The standard SPE cleanup approach uses a dual layer cartridge containing graphitized carbon (GCB) and PSA. In this application, Supelclean Ultra 2400 was used for SPE cleanup of chamomile extracts. Supelclean Ultra offers several advantages over the standard cartridge: (1) smaller size and thus less solvent usage, (2) does not require the use of toluene for elution, and (3) better recovery of pesticides with planar structures.
Featured Industry Food and Beverages
Legal Information Supelclean is a trademark of Sigma-Aldrich Co. LLC, SLB is a registered trademark of Sigma-Aldrich Co. LLC
Other Notes Clean-up process:
Cartridge: Top 3 mL Supelclean Ultra 2400 SPE cartridge (54281-U) with ~0.10 g anhydrous sodium sulfate
Condition: 3 mL of acetonitrile
Load: 750 μL of QuEChERS extract
Elute: using 8 mL of acetonitrile containing 0.5% formic acid, apply slight vacuum at end if needed.
Collect eluent in glass or plastic centrifuge tubes (glass preferred)
Concentrate: all eluent extracts in water bath at 45-50°C w/3 psi nitrogen purge to ~50-100 μL.
suitability application for GC/MS

Materials

     
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