Sensitive quantification of 5F-NNEI and characterization of its several metabolites in authentic urine and/or serum specimens obtained from three individuals by LC-QTRAP-MS/MS and high-resolution LC-Orbitrap-MS/MS
Sensitive quantification of 5F-NNEI and characterization of its several metabolites in authentic urine and/or serum specimens obtained from three individuals by LC-QTRAP-MS/MS and high-resolution LC-Orbitrap-MS/MS
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通过 LC-QTRAP-MS/MS 和高分辨率 LC-Orbitrap-MS/MS 对从三个个体获得的真实尿液和/或血清样本中的 5F-NNEI 进行灵敏定量及其几种代谢物的表征
DOI：
10.1007/s11419-018-0429-6
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发表时间：
2018
影响因子：
2.2
通讯作者：
Kanako Watanabe
中科院分区：
文献类型：
--
作者：
Kayoko Minakata;Hideki Nozawa;Itaru Yamagishi;Koutaro Hasegawa;Takeji Saitoh;Atsuto Yoshino;Masako Suzuki;Takuya Kitamoto;Osamu Suzuki;Kanako Watanabe
目的合成大麻素5 F-NNEI及其代谢产物在真实人体标本中的研究尚未见报道。本研究的目的是，首先，建立一个灵敏的定量方法，5 F-NNEI在人血清和尿液标本，其次，其代谢产物在真实的尿液标本从三个individuals.MethodsThese化合物的特征提取β-葡萄糖醛酸水解和未水解的尿液和/或血清标本通过液-液萃取。采用液相色谱（LC）-QTRAP串联质谱（MS/MS）进行鉴定和定量，并采用LC-高分辨-MS/MS对代谢产物进行表征。结果血清中5 F-NNEI的检测限为6 pg/mL，定量范围为10-2000 pg/mL，尿液中5 F-NNEI的检测限为3 pg/mL，定量范围为5-1000 pg/mL。设计的方法被应用于定量5 F-NNEI在真实的血清和/或尿液标本从三个人。例1和例2的血清5 F-NNEI水平分别为11.6和3680 pg/mL，例2和例3的尿5 F-NNEI水平分别为5.07和7.90 pg/mL。通过酰胺水解，脱乙酰，羟基化，羧化和/或葡萄糖醛酸化产生的5 F-NNEI的几种代谢产物，初步确定在尿液标本中的LC-高分辨率-MS/MS。ConclusionsA合成大麻素，5 F-NNEI，被确定和定量在其不变的形式，和它的几种代谢产物被初步确定在真实的标本从三个人，第一次到我们的知识。
PurposeA synthetic cannabinoid 5F-NNEI and its metabolites in authentic human specimens have not been reported yet. The aim of this study is, firstly, to establish a sensitive quantification method of 5F-NNEI in human serum and urine specimens, and, secondly, the characterization of its metabolites in authentic urine specimens obtained from three individuals.MethodsThese compounds were extracted from β-glucuronide-hydrolyzed and unhydrolyzed urine and/or serum specimens via liquid-liquid extraction. The identification and quantification were performed using liquid chromatography (LC)–QTRAP tandem mass spectrometry (MS/MS), and the characterization of the metabolites was done using LC–high-resolution-MS/MS.ResultsThe limits of detection for unchanged 5F-NNEI were 6 pg/mL with the quantification range of 10–2000 pg/mL in serum, and 3 pg/mL with the quantification range of 5–1000 pg/mL in urine. The devised method was applied to quantify 5F-NNEI in authentic serum and/or urine specimens from three individuals. The levels of 5F-NNEI were 11.6 and 3680 pg/mL in serum specimens of cases 1 and 2, respectively, and were 5.07 and 7.90 pg/mL in urine specimens of cases 2 and 3, respectively. Several metabolites of 5F-NNEI produced by amide hydrolysis, defluorination, hydroxylation, carboxylation and/or glucuronization were tentatively identified in the urine specimens by the LC–high-resolution-MS/MS.ConclusionsA synthetic cannabinoid, 5F-NNEI, was identified and quantified in its unchanged form, and its several metabolites were tentatively identified in authentic specimens obtained from three individuals, for the first time to our knowledge.