G1006927

LC/MS/MS Analysis of Pesticide Residues in Dates on the Ascentis^® Express RP-Amide Column after QuEChERS Extraction

application for LC-MS, application for SPE

Propiedades

• technique(s): LC/MS: suitable; solid phase extraction (SPE): suitable
• test parameters: sample/matrix: 5 g ground dates spiked with pesticides at 10 ng/g ; extraction process: add 10 mL water and 10 mL acetonitrile; shake 1 hr at 2500 rpm; add contents of Supel QuE citrate extraction tube (55227-U); . (shake for 1 minute; centrifuge at 5000 rpm fo 5 minutes and draw off supernatant); clean-up tube: Supel QuE PSA/C18 (55288-U); clean-up process: transfer 1 mL of the extract to 2 mLSupel QuE PSA/C18 tube; shake for 1 minute; centrifuge at 5000 rpm for 3 min; draw off supernatant for analysis.; sample preparation: Dilute 100 μL of cleaned extract to a final volume of 1 mL in 5 mM ammonium formate/0.1% formic acid in water; transfer diluted sample to vial for LC/MS/MS analysis ; column: Ascentis Express RP-Amide, 10 cm x 2.1 mm I.D., 2 μm particles (51576-U); mobile phase: (A) 5 mM ammonium formate with 0.1% formic acid in water; (B) 5 mM ammonium formate with 0.1% formic acid in 95:5 acetonitrile:H2O; gradient: held at 5% B from 0 to 1 min; to 100% B in 13 min; held at 100% B for 1.5 min; to 95% A in 0.5 min; held at 95% A for 1.5 min; flow rate: 0.4 mL/min; column temp.: 30 °C; detector: MS, ESI (+), MRM; injection: 5 μL
• suitability: application for LC-MS; application for SPE
• application(s): food and beverages

Descripción

Application

Freeze dates with liquid nitrogen and grind to a homogenous mixture.

Analysis Note

The “quick, easy, cheap, effective, rugged, and safe” (QuEChERS) method can be used to analyze multiple pesticide residues found in dates. In this study, QuEChERS extraction and cleanup using PSA/C18 were used for the analysis of pesticide residues of interest in pistachios. Average recoveries obtained for replicate samples spiked at 10 ng/g were in the range of 70-120% for 23 of the 25 pesticides analyzed.

Legal Information

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

Analito

Omethoate
Butocarboximsulfoxide
Aldicarb-sulfone
Methomyl
Carbendazim
Trichlorfon
Aldicarb
Thiacloprid
Thiophanate-methyl
Carbofuran
Methabenzthiazuron
Chlorantraniliprole
Spinetoram
Malathion
Bifenazate
Triazophos isomer#1
Triazophos isomer#2
Rotenone
Quinalphos
Etrimfos
Pyraflufen-ethyl
MGK-264 #1
MGK-264 #2
Neburon
Isoxathion
Spiromesifen
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