DOI: 10.1097/md.0000000000050058 ISSN: 0025-7974

Analytical method development and validation of a serum LC–MS/MS assay for 2 emerging synthetic cannabinoids

Murat Akbaba, Aysun Baransel Isir, Süleyman İbili, Can Erdem Yiğitsoy
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Background:

This study aimed to develop and validate a highly sensitive and reproducible liquid chromatography–tandem mass spectrometry (LC–MS/MS) method for the simultaneous determination of 5F-MDMB-PICA and MDMB-4en-PINACA in human serum, ensuring suitability for both forensic and clinical toxicology applications.

Methods:

Drug-free serum samples were fortified with target analytes, extracted through solid-phase extraction, and analyzed using a triple-quadrupole LC–MS/MS system (Shimadzu LCMS-8045) equipped with a biphenyl column. Calibration was established within 1–100 ng/mL, and validation parameters – linearity, sensitivity, accuracy, and precision – were assessed according to international guidelines.

Results:

The calibration curves displayed excellent linearity ( r 2  = 0.999) for both analytes. The limits of detection were 0.113 ng/mL for 5F-MDMB-PICA and 0.145 ng/mL for MDMB-4en-PINACA, with limits of quantification of 0.339 ng/mL and 0.435 ng/mL, respectively. Recovery rates at 10 and 50 ng/mL ranged from 77.7% to 96.4%, while intra and inter-day precision (relative standard deviation %) remained below 15%.

Conclusion:

The validated method provides reliable quantification of 5F-MDMB-PICA and MDMB-4en-PINACA in human serum. The observed linearity, sensitivity, recovery, and precision support its applicability for routine forensic toxicology analyses.

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