G1007604

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

suitable for GC/MS

Propiedades

• technique(s): GC/MS: suitable
• test parameters: 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 tube: Supelclean Ultra 2400, 3 mL (54281-U); clean-up process: See description text; 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); 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; carrier gas: helium, 1.4 mL/min constant flow; injection: 2 μL splitless; liner: 2 mm ID; sample: QuEChERS extract of chamomile
• application(s): food and beverages

Descripción

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.

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.

Legal Information

SLB is a registered trademark of Merck KGaA, Darmstadt, Germany

Supel is a trademark of Sigma-Aldrich Co. LLC

Supelclean is a trademark of Sigma-Aldrich Co. LLC

Analito

Naphthalene-d8 (QC std.)
Acenaphthene-d10 (QC std.)
Hexachlorobenzene
Quintozene
Atrazine
γ-BHC
Phenanthrene-d10 (QC std.)
Diazinon
Pentachloroaniline
Metalaxyl
PCB-52 (Int. std.)
Chlorpyrifos
Procymidone
α-Endosulfan
4,4’-DDE
ß-Endosulfan
Triazophos
Tris(1,3-dichloro-isopropyl)phosphate (Int. std.)
4,4’-DDT
Iprodione
Bifenthrin
Chrysene-d12 (QC std.)
cis-Permethrin
trans-Permethrin
Perylene-d12 (QC std.)
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