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

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

Materiales

Analytical column

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Ascentis® Express RP-Amide, 2 μm UHPLC Column

2 μm particle size, L × I.D. 10 cm × 2.1 mm

For use with

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Certified Vial Kit, Low Adsorption (LA), 2 mL, pk of 100

volume 2 mL, amber glass vial (with marking spot), natural PTFE/silicone septa (with slit), thread for 9 mm

Benchmixer XL multi-tube vortexer

AC/DC input 115 V AC

Standard

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Quinalphos

PESTANAL®, analytical standard

Rotenone

PESTANAL®, analytical standard

Aldicarb-sulfone

PESTANAL®, analytical standard

Etrimfos

PESTANAL®, analytical standard

Neburon

PESTANAL®, analytical standard

Omethoate

PESTANAL®, analytical standard

Butocarboximsulfoxide

PESTANAL®, analytical standard

Óxido de etileno solution

certified reference material, 50 mg/mL in methanol

Spiromesifen

PESTANAL®, analytical standard

Malathion

certified reference material, TraceCERT®

Carbendazim

certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland

Aldicarb

certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland

Methomyl

certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland

Thiacloprid

certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland

Carbofuran

reference material

Bifenazate

reference material

Chlorantraniliprole

reference material

Methabenzthiazuron

certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland

Triazophos

certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland

Trichlorfon

certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland

Spinetoram solution

100 μg/mL in acetonitrile, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland

Pyraflufen-ethyl

certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland

sample prep

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Supel QuE

Citrate Extraction Tube, pk of 50, suitable for EN 15662

Supel QuE

Empty Centrifuge Tube with Lid, centrifuge tube volume 50 mL, pk of 50, suitable for EN 15662:2008 per BS

Supel QuE

PSA/C18 Tube, pack of 100, AOAC® 2007.01

Supel QuE

PSA Tube, pk of 50, AOAC® 2007.01, centrifuge tube volume 15 mL , Shaker Compatible

substrate

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Glufosinate-ammonium

PESTANAL®, analytical standard

CONDITIONS

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

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