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 LC/MS/MS Analysis of Pesticide Residues in Pistachios](/deepweb/assets/sigmaaldrich/marketing/global/images/technical-documents/protocols/analytical-chemistry/quechers/g1006861-large/g1006861-large.jpg)
Figure 1.
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
Loading
Sign In To Continue
To continue reading please sign in or create an account.
Don't Have An Account?