Extraction of Phencyclidine (PCP) from Urine Using ISOLUTE® SLE+ Prior to GC/MS Analysis
Applications | 2014 | BiotageInstrumentation
The analysis of phencyclidine in urine is essential for forensic toxicology and clinical monitoring. Supported liquid extraction streamlines sample preparation, avoids emulsion issues, and enhances analyte recovery compared to traditional liquid–liquid extraction.
The primary goal was to develop and validate a rapid extraction method for PCP in urine using a supported liquid extraction platform followed by GC MS quantitation. The study assessed recovery, precision, and linearity across therapeutically and forensically relevant concentration ranges.
Urine samples were diluted with ammonium hydroxide and spiked with a deuterated PCP internal standard. Supported liquid extraction was performed on 1 mL sample columns using 1-chlorobutane as the eluent. Extracts were acidified with methanolic HCl, evaporated under air or nitrogen, and reconstituted in ethyl acetate prior to analysis.
Method recovery exceeded 88 percent across three donors with RSDs below 8 percent (n = 7). Calibration was linear from 10 to 1000 ng per milliliter with correlation coefficients above 0.999. The method LLOQ was established at 10 ng per milliliter.
Integration of supported liquid extraction into automated platforms and microelution formats is expected. Advances in mass spectrometry sensitivity and data processing will further enhance throughput and detection limits in toxicological screening.
The validated supported liquid extraction GC MS method provides a robust, reproducible, and high throughput solution for PCP analysis in urine, delivering excellent recovery, precision, and sensitivity for routine toxicology workflows.
Application Note AN829 Biotage 2014
GC/MSD, Sample Preparation, GC/SQ, Consumables
IndustriesClinical Research
ManufacturerAgilent Technologies, Biotage
Summary
Significance of Topic
The analysis of phencyclidine in urine is essential for forensic toxicology and clinical monitoring. Supported liquid extraction streamlines sample preparation, avoids emulsion issues, and enhances analyte recovery compared to traditional liquid–liquid extraction.
Objectives and Study Overview
The primary goal was to develop and validate a rapid extraction method for PCP in urine using a supported liquid extraction platform followed by GC MS quantitation. The study assessed recovery, precision, and linearity across therapeutically and forensically relevant concentration ranges.
Methodology
Urine samples were diluted with ammonium hydroxide and spiked with a deuterated PCP internal standard. Supported liquid extraction was performed on 1 mL sample columns using 1-chlorobutane as the eluent. Extracts were acidified with methanolic HCl, evaporated under air or nitrogen, and reconstituted in ethyl acetate prior to analysis.
Used Instrumentation
- Gas chromatograph Agilent 7890A with QuickSwap injector
- Column Agilent J W DB 5 30 m × 0.25 mm ID × 0.25 µm
- Carrier gas helium at 1.2 mL per minute
- Mass spectrometer Agilent 5975C operated in SIM mode monitoring key ions for PCP and PCP D5
Main Results and Discussion
Method recovery exceeded 88 percent across three donors with RSDs below 8 percent (n = 7). Calibration was linear from 10 to 1000 ng per milliliter with correlation coefficients above 0.999. The method LLOQ was established at 10 ng per milliliter.
Benefits and Practical Applications
- High extraction efficiency reduces processing time
- No emulsion formation simplifies workflow
- Sensitive quantitation down to 10 ng per milliliter
- Suitable for high throughput forensic and clinical laboratories
Future Trends and Potential Applications
Integration of supported liquid extraction into automated platforms and microelution formats is expected. Advances in mass spectrometry sensitivity and data processing will further enhance throughput and detection limits in toxicological screening.
Conclusion
The validated supported liquid extraction GC MS method provides a robust, reproducible, and high throughput solution for PCP analysis in urine, delivering excellent recovery, precision, and sensitivity for routine toxicology workflows.
Reference
Application Note AN829 Biotage 2014
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