Çift yönlü katı-faz ekstraksiyonu ve sıvı kromatografi-ardışık kütle spektrometresi ile kan örneklerinde sentetik kannabinoidlerin tayini

Abstract

AMAÇ: Son yıllarda kullanımı hızla artan sentetik kannabinoidlerin kan örneklerinde tayini için hassas ve güvenilir bir sıvı-kromatografisi ardışık kütle spektrometrik LC-MS/MS metot sunulması amaçlanmıştır.YÖNTEM: Kan örnekleri çift-yönlü katı faz ekstraksiyonu BDSPE ile ekstrakte edildikten sonra LC-MS/MS’e enjekte edilmiştir. Toplam olarak 57 adet sentetik kannabinoid ve metabolitleri Poroshell 2,7μm 150×4.6mm analitik kolonu ile gradiyent akış programı uygulanarak kantitatif olarak tayin edilmiştir. Metot validasyonu uluslararası rehberlere göre yapılmıştır. BULGULAR: Sadece 0,5mL kan örneği kullanılarak, tespit LOD ve tayin LOQ sınırları 0,3 ve 0,5ng/mL veya daha düşük olarak belirlenmiştir. Metot 0,5-100ng/mL arasında en düşük 0,990 belirleme katsayısı ile lineerdir. Geri kazanım oranları %54- %115 arasında ve ortalama %87’dir. Matriks etkisi analiz hassasiyetini negatif olarak etkilememekte, kesinlik ve doğruluk kabul edilebilir seviyelerdedir.SONUÇ: Her bir analitin düşük konsantrasyonlarda olsa bile tayinine imkân sağlayan metot adli ve klinik toksikoloji laboratuarlarının rutin uygulamalarında kullanılabilir.

Keywords

• Sentetik kannabinoid, adli toksikoloji, LC-MS/MS, metot validasyonu

An LC-MS/MS method for determination of synthetic cannabinoids in human blood using bidirectional solid-phase extractiont

Abstract

OBJECTIVE: To present a sensitive and reliable liquid chromatography–tandem mass spectrometry LC–MS/MS method for determination of synthetic cannabinoids in blood samples is aimed in this study. METHODS: The samples were prepared using a bidirectional solid phase extraction BD-SPE followed by injected to LC-MS/MS. A total of 57 synthetic cannabinoids and metabolites were separated on an Agilent Poroshell 2.7μm 150 × 4.6 mm column with gradient program and determined quantitatively. The method validation was done according to international guidelines.RESULTS: Limits of detection for all target analytes are 0.3 ng/mL or better, with only 0.5 mL of specimen used for analysis. The method is linear from 0.5 to 100 ng/mL with a correlation coefficient R2 greater than 0.990. Recovery values were in the ranges of 54.0% and 115.0% with a mean of 87%. Matrix effects did not negatively affect analytical sensitivity and precision and accuracy were acceptable at any quality control level.CONCLUSION: The method allowing the determination of each analyte, even at low concentrations, can be used in the routine applications of forensic and clinical toxicology laboratories.

Keywords

• Synthetic cannabinoid, forensic toxicology, LC-MS/MS, validation

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