Development of a chemometric method in urine sample for newly designed hallucinating psychoactive substances: 5-MeO-MiPT

Yıl 2023, Cilt: 62 Sayı: 3, 355 - 363, 18.09.2023

Ezgi Emen Rukiye Aslan Melike Aydoğdu Hasan Ertaş Serap Annette Akgür

https://doi.org/10.19161/etd.1360340

Cited By: 1

Öz

Aim: In this study, a method was developed for analysis and chemometric optimization for 5-methoxy-N-methyl-N-isopropyltryptamine (5-MeO-MiPT).
Materials and Methods: Our study was carried out in Ege University Institute on Drug Abuse, Toxicology and Pharmaceutical Science, Addiction Toxicology Laboratory.
Analysis and optimization of the effects of hydrolysis and solid phase extraction processes during the analysis of 5-MeO-MiPT by Gas Chromatography-Mass Spectrometry (GC-MS). For chemometric screenings design, Plackett-Burman was used. The most effective three factors were determined, and a central composite design was applied, and results were evaluated with surface response methodology. The method was validated for selectivity, linearity, the limit of detection, the limit of quantitation, accuracy, intra-day and inter-day repeatability, stability and carry over.
Results: In the chemometric method, the most effective parameters were found sample volume, hydrolysis temperature, and elution volume for 5-MeO-MiPT in urine analysis. Optimum values for these parameters were calculated by surface response methodology and the results were determined 1ml urine volume, 30°C hydrolysis temperature, 3,5 ml elution volume, respectively. The optimized method was validated for selectivity, linearity (25-500 ng/mL), limit of detection (5 ng/mL), limit of quantitation (18 ng/mL), accuracy (72-101%), intra-day and inter-day precisions were measured, respectively (4,43% RSD),(4,27% CV), stability and carry over parameters.
Conclusion: With a chemometric approach, quick, practical and accurate method for the detection of 5-MeO-MiPT has been developed with GC-MS. Working of 5-MeO-MiPT without derivatization in GC-MS analysis has shortened the pre-preparation time and is a pioneer for other analogs. It provides an effective method in the analysis of substances such as synthetic analogues from tryptamines which are added every day, with the use of such classical equipment and new methods.

Anahtar Kelimeler

5-MeO-MiPT, forensic toxicology; Gas Chromatography-Mass Spectrometry, solid-phase extraction, chemometry.

Halüsinasyon yapan yeni tasarım psikoaktif maddelerden biri olan 5-MeO-MiPTin idrarda tayinine yönelik kemometrik yöntem geliştirilmesi

Öz

Amaç: Bu çalışmada yeni psikoaktif maddelerden biri olan 5-metoksi-N-metil-N-izopropiltriptamin (5-MeO-MiPT) için analiz ve kemometrik optimizasyon için bir yöntem geliştirmeyi amaçladık.
Gereç ve Yöntem: Çalışmamız Ege Üniversitesi Madde Bağımlılığı, Toksikoloji ve İlaç Bilimleri Enstitüsü Bağımlılık Toksikolojisi Laboratuvarında gerçekleşmiştir. 5-MeO-MiPT'nin Gaz Kromatografi-Kütle Spektrometrisi (GC-MS) ile analizi sırasında hidroliz ve katı faz ekstraksiyon işlemlerinin etkileri incelendi ve optimizasyonu yapıldı. Kemometrik tarama tasarımı için Plackett-Burman kullanıldı. En etkili üç faktör belirlenerek merkezi bir kompozit tasarım uygulandı ve sonuçlar yüzey tepki metodolojisi ile değerlendirildi. Yöntem, seçicilik, doğrusallık, tespit limiti, miktar tayini limiti, doğruluk, gün içi ve günler-arası tekrarlanabilirlik, stabilite ve taşıma arasında valide edildi.
Bulgular: Kemometrik yöntemde, idrar analizinde 5-MeO-MiPT için en etkili parametreler numune hacmi, hidroliz sıcaklığı ve elüsyon hacmi bulundu. Bu parametreler için optimum değerler yüzey tepki metodolojisi ile hesaplandı ve sonuçlar sırasıyla 1 ml idrar hacmi, 30°C hidroliz sıcaklığı, 3,5 ml elüsyon hacmi olarak belirlendi. Optimize edilmiş yöntem seçicilik, doğrusallık (25-500ng/mL), belirtme alt limiti (5,63 ng/mL), tayin alt limiti 18,75 ng/mL), doğruluk (%43,01-%101,47), gün içi tekrarlanabilirlik ( 100 ng/ml derişimde 3 paralel, %RSD 4,43),günler-arası tekrarlanabilirlik (100 ng/ml derişimde 5 farklı gün 3 tekrarda, %CV 4,27), seyreltme tamlığı, taşınma etkisi ve kararlılık parametreleri incelenmiştir.
Sonuç: Kemometrik bir yaklaşımla, GC-MS ile 5-MeO-MiPT tespiti için hızlı, pratik ve doğru bir yöntem geliştirildi. 5-MeO-MiPT'nin GC-MS analizinde türevlendirilmeden çalışması, ön hazırlık süresini kısaltmış ve diğer analoglar için öncü olmuştur. Her gün eklenen triptaminlerin sentetik analogları gibi maddelerin analizinde bu tür klasik cihazlar/sistemler ve yeni yöntemler ile etkin bir yöntem sağlar.

Anahtar Kelimeler

5-MeO-MiPT, adli toksikoloji; Gaz Kromatografisi-Kütle Spektrometrisi, katı faz ekstraksiyonu, kemometri.

Kaynakça

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