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

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

Conditions

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
sample/matrix 5 g ground pistachios spiked with pesticides at 10 ng/g
extraction tube PK50 Supel QuE Citrate (EN) Tube (55227-U)
extraction process add 10 mL water and 10 mL acetonitrile; shake for 1 hour at 2500 rpm; add contents of Supel QuE citrate extraction tube; shake for 1 minute; centrifuge at 5000 rpm fo 5 minutes; draw off supernatant.
clean-up process transfer 1 mL of extract to 2 mL tube containing 75 mg Z-Sep+; shake for 1 minute; centrifuge at 5000 rpm for 3 minutes; draw off supernatant.
clean-up tube Supel QuE Z-Sep + (55408-U)
column Ascentis Express RP-Amide, 10 cm x 2.1 mm I.D., 2 µm particles (51576-U)
column temp. 30 C
mobile phase [A] 5 mM ammonium formate + 0.1% formic acid in water; [B] 5 mM ammonium formate + 0.1% formic acid in 95:5 acetonitrile:H2O
gradient 95% A 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
injection 5 µl
detector MS, ESI (+), MRM

Description

Analysis Note The quick, easy, cheap, effective, rugged, and safe (QuEChERS) method can be used to analyze µltiple pesticide residues found in pistachios. Because they contain a significant amount of fat, a cleanup step should be used as part of the QuEChERS method. In this study, QuEChERS extraction and cleanup using Z-Sep+ was 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. .
Featured Industry Food and Beverages
Legal Information Ascentis is a registered trademark of Sigma-Aldrich Co. LLC
Other Notes Freeze whole pistachios (with shells) using liquid nitrogen, and grind.
suitability application for LC-MS, application for SPE

Materials

     
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