Screening and Quantitation of 250 Pesticides in Apple, Cranberry, Orange, Vegetable and White Grape Juices using the eXtreme|FV® by LC/MS/MS

Z.Yang, L. Maljers, Bruker, Chemical & Applied Markets (CAM) Division. “Screening and Quantitation of 250 Pesticides in Fruit Juices with Positive/Negative Switching LC/MS/MS.” Poster presented as part of NACRW-FPRW Conference, St. Petersburg, FL., 20-23 July 2014.

Abstract

A study was conducted using the Bruker EVOQ for the analysis of 250 pesticides in store-bought juice using one method and simple sample preparation using the Thomson eXtreme|FV®s in a dilute-and-shoot approach without sample enrichment. LC-MS/MS operated in Multiple Reaction Monitoring (MRM) mode with dual scan Electrospray Ionization (ESI) is widely used for polar, semi-volatile, and thermally labile pesticides in food testing. The Bruker EVOQ Elite LC-Triple Quadrupole System provides fast positive/negative switching, allowing for simultaneous determination of positive and negative co-eluting compounds numbering in the hundreds. Simple sample preparation is explored using Thomson eXtreme|FV®s for sample clean-up instead of lengthy alternatives like SPE or centrifugation followed by liquid-liquid extraction.

Equipment

  • EVOQ Elite Triple Quadrupole Mass Spectrometer
  • Bruker UHPLC
  • CTC Autosampler
  • Source: HESI
  • Spray Voltage Positive: 4000V
  • Spray Voltage Negative: 4000V
  • Column: YMC-Pack ODS-AQ 3μm
  • Column Temperature: 40°C
  • Injection Volume: 30μL
  • Mobile Phase:
    • Mobile Phase A: 5mM Ammonium Fluoride in Water
    • Mobile Phase B: Methanol
    • Gradient:
      • Time%A%BFlow (μL/min)
        0.009010400
        0.209010400
        2.003070400
        10.00100400
        15.00100400
        15.19010500
        18.09010400

Sample Preparation

  1. Pipette 50μL of store-bought apple juice and 450μL of solvent (10% Methanol/ 90% Water) directly into the outer shell of Thomson eXtreme|FV®, 0.2μm PVDF.
  2. Partially depress the eXtreme|FV® plunger and vortex.
  3. Depress the completely and load onto the autosampler.

Results

Table.1Store bought fruit juice test results
Fuit JuiceApple JuiceOrange JuiceCranberry JuiceWhite Grape JuiceVegetable Juice
Pesticideµg/L (ppb)
AzoxystrobinNDND0.32ND0.48
BoscalidNDND0.16NDND
CarbarylND0.391.47NDND
CarbofuranND0.14NDNDdND
DimethoateND0.30NDNDND
ImidaclopridNDND0.60ND0.20
MandipropanidNDND0.59NDND
MetalaxylNDND0.21NDND
MethoxyfenozideNDNDNDND0.84
TebuconazoleNDND0.32NDND
Thiabenazole1.8NDNDNDND
fruit juice chromatograms

fig.1Fig 1. Chromatogram of a 0.01ppb standard solution containing the compounds listed in Table 1 This is equivalent to 0.1ppb in juice.

fruit juice calibration curves

fig.2Calibration curve of negative pesticide Fipronil (left top) and positive pesticide Cyazofamid (left bottom), and their co-eluting plots (right).

fruit juice total ion chromatograms

fig.3Total Ion Chromatograms for all juices

Conclusion

The calibration on triplicate injections showed excellent linearity and response factor RSD over 3 orders, range using the Thomson eXtreme|FV® for sample preparation. Pesticides were detected in store-bought apple, orange, cranberry and vegetable juices.

  • Good linearity
  • sensitivity and response factor
  • RSD for positive and negative co-eluting pesticides

Title

Screening and Quantitation of 250 Pesticides in Apple, Cranberry, Orange, Vegetable and White Grape Juices using the eXtreme|FV® by LC/MS/MS

Description

[A]nalysis of 250 pesticides in store-bought juice using one method and simple sample preparation using the Thomson [eXtreme|FV®] in a dilute-and-shoot approach without sample enrichment ... sample preparation is explored using eXtreme|FV® for sample clean-up instead of lengthy alternatives like SPE or centrifugation followed by liquid-liquid extr...

PDF Application

Product Used in Application

eXtreme|FV® - PVDF 0.2µm

Pre-Split Septum, Red Cap

pn#85531-200

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