Routine Targeted Quantitation & Identification of Pesticide Residues in Avocado, Carrot, Grape & Orange using the eXtreme|FV® by LC-MS/MS

Schreiber, AB SCIEX, Concord, ON, Canada; J. Jasak, AB SCIEX, Darmstadt, Germany. “Routine Targeted Quantitation and Identification of Pesticide Residues using Triple Quadrupole LC-MS/MS and Advanced Scheduling of MRM Transitions” Poster presented as part of NACRW-FPRW Conference, St. Petersburg, FL., 20-23 July 2014.

Introduction

LC-MS/MS is a powerful analytical tool capable of screening samples for numerous compounds. MRM is typically used because of its excellent sensitivity, selectivity, and speed. Using QuEChERS for extraction, eXtreme|FV®s for clean-up, and UHPLC combined with core-shell particles columns provides good resolution and excellent peak shape, making it possible to detect hundreds of pesticides of a wide variety of compound classes and chemical properties in each sample. The new AB SCIEX Triple Quad™ 3500 with a Turbo V™ source and Curtain Gas™ interface supplies exceptional robustness and ruggedness. The advanced eQ™ electronics and the curved LINAC® collision cell were designed for unparalleled speed of MRM detection and fast polarity switching for comprehensive multi-component analysis. The method combines QuEChers for extraction, Thomson eXtreme|FV®s for clean-up, and the Sciex Scheduled MRM Pro Algorithm for identification of pesticides in fruit and vegetables analysis.

Equipment

  • AB Sciex Triple Quad™ 3500 with Turbo V™ source and Electrospray Ionization Positive Polarity
  • Column: Phenomenex Kinetex™ Biphenyl 2.6μm column
  • Mobile Phase: Fast gradient of Water/Methanol with 5mM Ammonium Formate
    • Flow rate: 0.5mL/min
      • StepTime(min)A(%)B(%)
        00.09010
        10.59010
        22.07030
        39.04060
        411.02080
        512.0595
        615.0595
        716.09010
        820.09010

Sample Preparation

  1. Store-bought Avocado, Carrot, Grape & Orange is extracted using dispersive SPE following the European Standard Method 15662
  2. SCIEX iDQuant™ standards kit are used for Pesticide Analysis
  3. Extracts are diluted and filtered 5x with water in Thomson eXtreme|FV®, 0.45μm PVDF membrane

Results

veggie sensitivity of selected pesticides

fig.1Fig 1. Sensitivity of selected pesticides detected at a concentration of 5ng/mL using the Triple Quad™ 3500 system (click image for larger)

veggie calibration curves

fig.2Fig 2. Calibration line of Azoxystrobin from 0.1 to 100 ng/mL (top) and quantifier-qualifier ratio for compound identification (bottom).

SamplePesticideConcentration (μg/kg)MRM Ratio (Expected Ratio)
AvocadoAzoxystrobin55.00.146 (0.126)
Imidacloprid6.20.823 (0.818)
Thiabendazole2.91.035 (0.820)
CarrotLinuron14.30.613 (0.742)
Thiabendazole5.30.995 (0.820)
GrapesBoscalid17.30.240 (0.242)
Fenhexamid3630.973 (1.053)
Methamidophos1.20.873 (0.698)
Myclobutanil14.20.811 (0.830)
Pyrimethanil6870.482 (0.435)
Tebuconazole7.10.030 (0.261)
OrangeImazalil18300.282 (0.348)
Thiabendazole>30000.812 (0.820)
SpinachBoscalid12.30.264 (0.242)
Dimethomorph53.70.537 (0.541)
Fenamidone7550.749 (0.672)
Imidacloprid2170.907 (0.993)
Propamocarb3.10.260 (0.336)
Thiabendazole3.60.917 (0.820)

Conclusion

  • The AB Sciex Triple Quad 3500 was used for pesticide residue identification and quantification in store-bought fruit and vegetables.
  • Method combines QuEChers extraction, Thomson eXtreme|FV®s, Phenomenex Kintex Biphenyl Column, and the Sciex Scheduled MRM Pro Algorithm.
  • Average gain in sensitivity of 3x was observed, with most pesticides having an LOD of < 1ng/mL.

Title

Routine Targeted Quantitation & Identification of Pesticide Residues in Avocado, Carrot, Grape & Orange using the eXtreme|FV® by LC-MS/MS

Description

Thomson eXtreme|FV®s for clean-up, and the Sciex Scheduled MRM Pro Algorithm for identification of pesticides in fruit and vegetables analysis.

PDF Application

Product Used in Application

eXtreme|FV® - PVDF 0.45µm

eXtreme|FV® - PVDF 0.45µm

Pre-Split Septum, Yellow Cap

pn#85541-200

Related Products

© 2021 Thomson |
Solutions At Work™

LinkedIn