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

Yıl 2017, Cilt: 31 Sayı: 3, 101 - 114, 01.12.2017

Oya Yeter

Öz

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.

Anahtar Kelimeler

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

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

Öz

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.

Anahtar Kelimeler

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

Kaynakça

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