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1 2017

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Fast confirmation for marijuana metabolite: THC-COOH, ultra-fast LC—MS/MS run time, and application to routine samples

Zazoğlu S., Anilanmert B., Aydin M., Cengiz S.

Acta Chromatographica

2017

Vol. 29, no. 2

253--265

A fast, reliable, inexpensive, and practical method with a low determination limit and high recovery has been developed for the determination of the marijuana metabolite in routine analysis. THC-COOH in urine was validated using liquid chromatography—tandem mass spectrometry (LC—MS/MS). Before an easy single-step extraction with Toxi-Tubes, basic hydrolysis was performed at 60 °C for 30 min. LC—MS/MS analysis takes 2.5 min for each sample, and the retention time of the analyte is 1.75 min. Specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, repeatability, and intermediate precision (inter-day) system suitability parameters were determined in the validation study. The recovery of the extraction method was 88.67 (±5.91). LOD and LOQ values were 1.41 and 5.00 ng mL−1, respectively. The method showed linear response between the values 5.00 and 500.00 ng mL−1. The repeatability was 9.64% (relative standard deviation, RSD%), and the intermediate precisions (RSDR%) were 10.73%, 13.74%, and 8.11% at 10.00, 100.00, and 200.00 ng mL−1 concentration levels, respectively. No statistically significant difference was found in ANOVA analysis, between three consecutive days in intermediate precision study, for 90% confidence level. HorRat values were between 0.34 and 0.61. The method was applied to CEDIA positive samples, obtained from the Trabzon Group Presidency of Turkish Council of Forensic Medicine, successfully.