Simple, Fast, and Clean Extraction of Synthetic Cannabinoids from Whole Blood Using Oasis PRiME HLB
Applications | 2015 | WatersInstrumentation
The analysis of synthetic cannabinoids in biological matrices is critical for forensic toxicology, clinical diagnostics, and regulatory compliance. Rapid and reliable sample preparation that minimizes matrix interferences and maximizes throughput is essential for monitoring emerging designer drugs in whole blood.
This study aimed to develop a streamlined solid-phase extraction (SPE) method for 22 synthetic cannabinoids and their major metabolites in whole blood. The goals were to eliminate conditioning steps, achieve high recoveries, reduce phospholipid contamination, and deliver robust quantitative performance using Oasis PRiME HLB sorbent.
A simple load-wash-elute protocol was applied without conditioning or equilibration. Blood samples were lysed with zinc sulfate/ammonium acetate, precipitated with acetonitrile, and the supernatant diluted prior to direct loading on 30 mg Oasis PRiME HLB plates. After washing with 25:75 MeOH:water and elution with 90:10 ACN/MeOH, extracts were evaporated and reconstituted in 30% ACN.
Used Instrumentation:
Chromatography was completed in 7.5 min with sharp, symmetric peaks. Average extraction recovery was 91% (RSD ~5%), and mean matrix effect was 17% across all analytes. Phospholipid removal exceeded 95% compared to protein precipitation, yielding cleaner extracts and likely extending column and source lifetimes. Calibration curves were linear (r2 ≥0.99 for 21/22 compounds), and QC samples at 2.5, 7.5, and 75 ng/mL demonstrated accuracies within 85–110% and RSDs below 15%. LLOQs ranged from 0.1 to 1 ng/mL without deuterated internal standards.
With the continuous emergence of new synthetic cannabinoids, this universal SPE approach promises rapid method adaptation. Integration with automated 96-well workflows and high-resolution mass spectrometry could further enhance throughput and expand target panels. Advanced sorbents may enable simultaneous screening for additional drug classes in complex matrices.
The Oasis PRiME HLB µElution method provides a fast, clean, and high-throughput solution for extracting synthetic cannabinoids from whole blood. It delivers consistent high recoveries, minimal matrix effects, and over 95% phospholipid removal, supporting reliable quantitative analysis without extensive sample preparation steps.
Danaceau J. P., Chambers E. E., Fountain K. J. Analysis of synthetic cannabinoids from urine for forensic toxicology using Oasis HLB µElution plates and CORTECS UPLC columns. Waters Application Note. 2015;
Sample Preparation, Consumables, LC/MS, LC/MS/MS, LC/QQQ
IndustriesForensics
ManufacturerWaters
Summary
Importance of the Topic
The analysis of synthetic cannabinoids in biological matrices is critical for forensic toxicology, clinical diagnostics, and regulatory compliance. Rapid and reliable sample preparation that minimizes matrix interferences and maximizes throughput is essential for monitoring emerging designer drugs in whole blood.
Objectives and Study Overview
This study aimed to develop a streamlined solid-phase extraction (SPE) method for 22 synthetic cannabinoids and their major metabolites in whole blood. The goals were to eliminate conditioning steps, achieve high recoveries, reduce phospholipid contamination, and deliver robust quantitative performance using Oasis PRiME HLB sorbent.
Methodology and Instrumentation
A simple load-wash-elute protocol was applied without conditioning or equilibration. Blood samples were lysed with zinc sulfate/ammonium acetate, precipitated with acetonitrile, and the supernatant diluted prior to direct loading on 30 mg Oasis PRiME HLB plates. After washing with 25:75 MeOH:water and elution with 90:10 ACN/MeOH, extracts were evaporated and reconstituted in 30% ACN.
Used Instrumentation:
- Oasis PRiME HLB 30 mg plates
- CORTECS UPLC C18 column (2.1×100 mm, 1.6 µm)
- ACQUITY I-Class UPLC system
- Xevo TQD triple quadrupole mass spectrometer
Main Results and Discussion
Chromatography was completed in 7.5 min with sharp, symmetric peaks. Average extraction recovery was 91% (RSD ~5%), and mean matrix effect was 17% across all analytes. Phospholipid removal exceeded 95% compared to protein precipitation, yielding cleaner extracts and likely extending column and source lifetimes. Calibration curves were linear (r2 ≥0.99 for 21/22 compounds), and QC samples at 2.5, 7.5, and 75 ng/mL demonstrated accuracies within 85–110% and RSDs below 15%. LLOQs ranged from 0.1 to 1 ng/mL without deuterated internal standards.
Benefits and Practical Applications
- Greatly simplified SPE workflow by removing conditioning/equilibration
- High recoveries and low variability without internal standards
- Efficient phospholipid depletion to improve data quality and instrument uptime
- Universal applicability to neutral, acidic, and basic synthetic cannabinoids and metabolites
Future Trends and Opportunities
With the continuous emergence of new synthetic cannabinoids, this universal SPE approach promises rapid method adaptation. Integration with automated 96-well workflows and high-resolution mass spectrometry could further enhance throughput and expand target panels. Advanced sorbents may enable simultaneous screening for additional drug classes in complex matrices.
Conclusion
The Oasis PRiME HLB µElution method provides a fast, clean, and high-throughput solution for extracting synthetic cannabinoids from whole blood. It delivers consistent high recoveries, minimal matrix effects, and over 95% phospholipid removal, supporting reliable quantitative analysis without extensive sample preparation steps.
Reference
Danaceau J. P., Chambers E. E., Fountain K. J. Analysis of synthetic cannabinoids from urine for forensic toxicology using Oasis HLB µElution plates and CORTECS UPLC columns. Waters Application Note. 2015;
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