GC/MSD, GC/MS/MS, Sample Preparation, GC/QQQ, GC/API/MS, LC/MS, LC/MS/MS, LC/QQQ
IndustriesFood & Agriculture
ManufacturerAgilent Technologies, Waters
Significance of the topic
Chlorophyll and other pigments co-extracted during QuEChERS sample preparation can severely compromise GC-MS/MS and UPLC-MS/MS instrument performance. Effective removal of these interferences is essential to prolong column life, maintain signal stability, and ensure accurate quantitation of pesticides in high-pigment matrices such as spinach.
Aims and overview of the study
This work evaluates the performance of Oasis PRiME HLB cartridges in Vac and Plus formats for rapid, pass-through cleanup of chlorophyll from spinach QuEChERS extracts. The cartridges are compared to conventional dispersive SPE using graphitized carbon black (GCB) at different loadings, focusing on pigment removal and recovery of planar pesticides.
Methodology and instrumentation
Spinach samples spiked with 50 µg/kg of planar pesticides (cyprodinil, chlorothalonil, thiabendazole) underwent QuEChERS extraction. Cleanup strategies included:
- dSPE with 10 mg or 50 mg GCB per mL extract alongside standard sorbents
- Pass-through cleanup using Oasis PRiME HLB cartridges (Vac style, Plus Light, Plus Short) without conditioning
- APGC-MS/MS (Xevo TQ-S) for cyprodinil and chlorothalonil on an Agilent 7890 GC and Restek Rxi-5ms column
- UPLC-MS/MS (Xevo TQ-S micro) for thiabendazole on an ACQUITY UPLC I-Class system with BEH C18 column
Mobile phases, temperature programs, and ion transitions were optimized for each platform.
Main results and discussion
Pass-through cleanup with Oasis PRiME HLB cartridges removed over 99% of chlorophyll and over 95% of lutein, outperforming dSPE with 10 mg GCB. While dSPE with 50 mg GCB achieved complete pigment removal, it caused significant losses of planar pesticides. Oasis PRiME HLB maintained analyte recoveries with minimal loss and showed consistent performance across different cartridge formats.
Benefits and practical applications
The Oasis PRiME HLB pass-through approach simplifies workflow by eliminating conditioning steps, reduces matrix-related interferences, and preserves recoveries of sensitive planar analytes. Its compatibility with syringes and vacuum manifolds allows flexible integration into routine pesticide analysis in high-pigment commodities.
Future trends and possibilities
Expansion of pass-through sorbent technology could address cleanup challenges in other complex matrices (e.g., leafy greens, fruits with high chlorophyll content). Integration with automated platforms and adaptation for broader analyte panels will further enhance throughput and sustainability in food safety testing.
Conclusion
Oasis PRiME HLB cartridges provide a rapid and effective pass-through cleanup solution for chlorophyll-rich QuEChERS extracts, offering superior pigment removal and analyte recovery compared to traditional dSPE with GCB. Their ease of use and robust performance support reliable pesticide monitoring in challenging matrices.
Reference
Oasis PRiME HLB Cartridge for Rapid and Effective Cleanup of Avocado, A High Fat Matrix, Prior to APGC-MS/MS Analysis, Waters Application Note 720005816EN, 2016.
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