Quantification of 75 Synthetic Cannabinoids in Seized E-liquid Samples by <sup>1</sup>H qNMR

LIU Cui-mei; JIA Wei; SONG Chun-hui; HUA Zhen-dong

doi:10.19969/j.fxcsxb.23010403

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Quantification of 75 Synthetic Cannabinoids in Seized E-liquid Samples by ¹H qNMR

Scientific Papers | 更新时间：2023-05-15

- Quantification of 75 Synthetic Cannabinoids in Seized E-liquid Samples by ¹H qNMR
- Journal of Instrumental Analysis Vol. 42, Issue 5, Pages: 605-613(2023)
- 作者机构：
  
  1.公安部禁毒情报技术中心毒品监测管控与禁毒关键技术公安部重点实验室，北京 100193
  2.中国药科大学药学院，江苏南京 210009
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.23010403
  CLC：
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刘翠梅,贾薇,宋春辉等.缴获电子烟油样品中75种合成大麻素的¹H qNMR定量分析研究[J].分析测试学报,2023,42(05):605-613.

LIU Cui-mei,JIA Wei,SONG Chun-hui,et al.Quantification of 75 Synthetic Cannabinoids in Seized E-liquid Samples by ¹H qNMR[J].Journal of Instrumental Analysis,2023,42(05):605-613.
刘翠梅,贾薇,宋春辉等.缴获电子烟油样品中75种合成大麻素的¹H qNMR定量分析研究[J].分析测试学报,2023,42(05):605-613. DOI： 10.19969/j.fxcsxb.23010403.

LIU Cui-mei,JIA Wei,SONG Chun-hui,et al.Quantification of 75 Synthetic Cannabinoids in Seized E-liquid Samples by ¹H qNMR[J].Journal of Instrumental Analysis,2023,42(05):605-613. DOI： 10.19969/j.fxcsxb.23010403.

摘要

通过考察75种合成大麻素（SCRAs）的关键定量参数，首次建立了可用于电子烟油样品中75种SCRAs定量分析的核磁共振氢谱定量分析方法（,1,H qNMR）。以1，3，5-三甲氧基苯为内标，将烟油样品经氘代甲醇稀释后直接进行分析。方法的定量下限为0.03%（质量分数），日内相对标准偏差（RSD）小于0.90%，日间RSD小于1.5%，基质加标回收率为93.3% ~ 100%。采用,1,H qNMR法对19份缴获烟油样品中的4种合成大麻素3，3-二甲基-2-［1-（5-氟戊基）吲唑-3-甲酰氨基］丁酸甲酯（5F－ADB）、2-［1-（5-氟戊基）-1H-吲哚-3-甲酰氨基］-3，3-二甲基丁酸甲酯（5F－MDMB－PICA）、2-［1-（4-氟丁基）-1H-吲唑-3-甲酰氨基］-3，3-二甲基丁酸甲酯（4F－MDMB－BUTINACA）、N-（1-氨基-3，3-二甲基-1-氧代丁-2-基）-1-丁基-1H-吲唑-3-甲酰胺（ADB－BUTINACA）进行定量分析，得到其含量范围为0.072% ~ 2.056%。19份烟油样品的,1,H qNMR定量结果与高效液相色谱法定量结果无显著性差异。该研究所建立的电子烟油中SCRAs的定量分析,1,H qNMR法无需标准物质，操作简单，定量结果准确，解决了缺乏标准物质时复杂基质中SCRAs定量分析的难题。目前国内外尚未有采用,1,H qNMR对电子烟油中75种SCRAs定量分析的报道。该研究进一步拓宽了,1,H qNMR技术在禁毒领域的应用范围，为复杂基质中毒品和新精神活性物质的定量分析提供了新的思路。

Abstract

A general ,1,H nuclear magnetic resonance spectroscopic（,1,H 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（,T,1,），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 ,1,H 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 ,1,H 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 ,1,H qNMR．This study further broadens the application scope of ,1,H qNMR in the field of drug control，and provides a new idea for quantitative analysis of drugs and new psychoactive substances in complex matrix.

关键词

电子烟油新精神活性物质（NPS）合成大麻素核磁共振氢谱定量分析

Keywords

e-liquidsnew psychoactive substances（NPS）synthetic cannabinoids1H quantitative nuclear magnetic resonance spectroscopy analysis（1H qNMR）

references

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College of Criminal Science and Technology，Nanjing Police College

Institute of Forensic Science，Public Security Bureau of Jiangyin，Jiangyin

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Quantification of 75 Synthetic Cannabinoids in Seized E-liquid Samples by 1H qNMR

DOI：10.19969/j.fxcsxb.23010403

摘要

Abstract

关键词

Keywords

references

Quantification of 75 Synthetic Cannabinoids in Seized E-liquid Samples by ¹H qNMR