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Merck

G1007604

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

suitable for GC/MS

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About This Item

テクニック

GC/MS: suitable

試験パラメータ

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

アプリケーション

food and beverages

アナリシスノート

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.

その他情報

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.

法的情報

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

アナライト

詳細

    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.)
    すべて表示 (25)

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