Development and validation of an LC-MS/MS method for determination of phencyclidine in human serum and its application to human drug abuse cases
2010
Chimalakonda, Krishna C. | Hailey, Chris | Black, Ryan | Beekman, Allison | Carlisle, Rebecca | Lowman-Smith, Elizabeth | Singletary, Heather | Owens, S Michael | Hendrickson, Howard
A new analytical method was developed and validated for the rapid determination of phencyclidine (PCP) in human blood and serum. Rapid chromatographic separation decreased the analysis time relative to standard gas chromatography (GC)-based methodologies. The method involved the use of solid-phase extraction for sample preparation and cleanup followed by liquid chromatography tandem spectrometric (LC-MS/MS) analysis and an electrospray-ionization (ESI) interface. PCP was quantified using multiple-reaction-monitoring with deuterium labeled PCP (PCP-d₅) as an internal standard. The method was validated for accuracy, precision, linearity, and recovery. The method was accurate with error <14% and precision with coefficient of variation (CV) <5.0%. The assay was linear over the entire range of calibration standards (r² > 0.997). The recovery of PCP after solid-phase extraction was greater than 90% with the lower limit of detection (LLOD) for PCP in 500 µl of human serum after solid-phase extraction at 0.06 ng ml⁻¹. This method was used to determine the levels of PCP in postmortem human blood samples. The LLOD in blood was 1 ng ml⁻¹. Blood PCP concentrations were also determined separately using GC and flame ionization detection (FID). Blood calibration standards and serum calibration standards yielded similar concentrations when used to quantitate authentic human blood samples that tested positive for PCP under the GC-FID method. Extraction of PCP from serum required fewer steps and therefore could be used as a calibration matrix in place of blood. The LC-MS/MS methodology shown here was higher throughput compared with GC-based methods because of very short chromatographic run times. This was accomplished without sacrificing analytical sensitivity.
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