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| Quantification of 75 Synthetic Cannabinoids in Seized E-liquid Samples by 1H qNMR |
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| DOI： |
| KeyWord:e-liquids new psychoactive substances（NPS） synthetic cannabinoids 1H quantitative nuclear magnetic resonance spectroscopy analysis（1H qNMR） |
| Author | Institution |
| LIU Cui-mei，JIA Wei，SONG Chun-hui，HUA Zhen-dong |
1. Key Laboratory of Drug Monitoring and Control，Drug Intelligence and Forensic Center，Ministry of Public Security，Beijing ，China; 2. School of Pharmacy，China Pharmaceutical University， Nanjing ，China |
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| Abstract: |
| A general 1H nuclear magnetic resonance spectroscopic（1H qNMR） method was established for the quantification of 75 synthetic cannabinoid receptor agonists（SCRAs） in seized e-liquid samples in this paper．The key qNMR spectrum acquisition and processing parameters，such as spin-lattice relaxation time（T1），internal standard and SCRAs quantitative peak were thoroughly discussed．1，3，5-trimethoxybenzene was used as the internal standard，and the samples were directly analyzed after dilution with deuterated methanol．The limit of quantitation（LOQ） of this method was 0.03%，the intra-day relative standard deviation（RSD） was less than 0.90%，the inter-day RSD was less than 1.5%，and the spiked recoveries for the matrixes were in the range of 93.3%－100%．The developed method was applied to the quantification of four SCRAs，including N-（1-methoxy-3，3-dimethyl-1-oxobutan-2-yl）-1-（5-fluoropentyl）-1H-indazole-3-carboxamide（5F－ADB），methyl 2-（1-（5-fluoropentyl）-1H-indole-3-carboxamido）-3，3-dimethylbutanoate（5F－MDMB－PICA），methyl 2-（1-（4-fluorobutyl）-1H-indazole-3-carboxamido）-3，3-dimethylbutanoate（4F－MDMB－BUTINACA），and N-（1-amino-3，3-dimethyl-1-oxobutan-2-yl）-1-butyl-1H-indazole-3-carboxamide（ADB－BUTINACA） in 19 seized e-liquid samples．The contents of SCRAs ranged from 0.072% to 2.056%．To be specific，the content of 5F－ADB ranged from 0.081% to 0.200%（n = 3），the content of 5F－MDMB－PICA ranged from 0.072% to 1.453%（n = 7），the content of 4F－MDMB－BUTINACA ranged from 0.122% to 0.477%（n = 5），and the content of ADB－BUTINACA ranged from 0.561% to 2.056%（n = 4）．The quantitative results for SCRAs in 19 e-liquids by 1H qNMR and high-performance liquid chromatography（HPLC） were compared using Wilcoxon signed-rank test．The test P value was 1.00，indicating that there was no significant difference between the quantitative results of these two methods．The proposed 1H qNMR method is simple and accurate，which does not require the SCRAs reference material．It solves the problem of quantitative analysis for SCRAs in complex matrix when there is no reference material．At present，there is no report on the quantitative analysis of 75 kinds of SCRAs in e-liquids by 1H qNMR．This study further broadens the application scope of 1H qNMR in the field of drug control，and provides a new idea for quantitative analysis of drugs and new psychoactive substances in complex matrix. |
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