低场^(1)H qNMR定量分析缴获毒品中氯胺酮及4种掺杂物  

Quantification of Ketamine and Four Kinds of Adulterants in Seized Drugs by Low-field ^(1)H Nuclear Magnetic Resonance Spectroscopy

作　　者：刘翠梅 宋春辉 贾薇 花镇东 廖琦 LIU Cui-mei;SONG Chun-hui;JIA Wei;HUA Zhen-dong;LIAO Qi(Key Laboratory of Drug Monitoring and Control,Drug Intelligence and Forensic Center,Ministry of Public Security,Beijing 100193,China;School of Pharmacy,China Pharmaceutical University,Nanjing 210009,China;Anti-drug Technology Center of Shaanxi Provincial Public Security Department,National Anti-drug Laboratory Shaanxi Regional Center,Xi’an 710115,China)

机构地区：[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 [3]国家毒品实验室陕西分中心陕西省公安厅毒品技术中心,陕西西安710115

出　　处：《分析测试学报》2023年第6期755-761,共7页Journal of Instrumental Analysis

基　　金：公安部科技计划项目(2021JC23);国家重点研发计划项目(2022YFC3300902)。

摘　　要：建立了可同时定量分析缴获毒品中氯胺酮、二甲基砜、磺胺、烟酰胺和非那西丁的低场氢谱核磁共振定量方法(LF-^(1)H qNMR),并将其定量能力与高场氢谱核磁共振定量方法(HF-^(1)H qNMR)进行了比较。对于LF-^(1)H qNMR,氯胺酮和4种掺杂物的日内相对标准偏差(RSD)、日间RSD和定量下限分别为0.50%~2.9%、2.0%~7.4%和0.3~5 mg/mL;对于HF-^(1)H qNMR,氯胺酮和4种掺杂物的日内RSD、日间RSD和定量下限分别为0.40%~1.1%、1.5%~3.9%和0.003~0.05 mg/mL。采用LF-^(1)H qNMR和HF-^(1)H qNMR对167份缴获氯胺酮样品进行定量分析,两种方法定量结果的相对误差均小于15%。LF-^(1)H qNMR测得氯胺酮、二甲基砜、磺胺、烟酰胺和非那西丁的纯度分别为13.5%~102.6%、1.1%~81.3%、2.6%~83.4%、1.8%~22.7%和3.4%~43.8%;HF-^(1)H qNMR测得的纯度分别为13.2%~99.7%、1.0%~78.4%、2.5%~75.9%、1.7%~21.3%和3.0%~43.5%。两种方法均可在不使用标准物质的情况下实现对氯胺酮和掺杂物的同时定量分析。虽然LF-^(1)H qNMR法的精密度和灵敏度略低于HF-^(1)H qNMR法,但其对复杂基质中多组分同时定量分析的能力较好。LF-^(1)H qNMR的仪器购置和日常维护费用远低于HF-^(1)H qNMR,未来将在法庭科学实验室中得到更广泛的应用。A low-field ^(1)H quantitative nuclear magnetic resonance(LF-^(1)H qNMR)spectroscopy was developed for the simultaneous quantification of ketamine and 4 adulterants,i.e.dimethyl sulfone,sulfanilamide,niacinamide,and phenacetin in this paper.Meanwhile,its quantification ability was compared with that of high-field 1H quantitative nuclear magnetic resonance(HF-^(1)H qNMR).As for LF-^(1)H qNMR,the intra-day relative standard deviations(RSDs),inter-day RSDs,and lim⁃it of quantitations(LOQs)for ketamine and 4 adulterants were in the range of 0.50%-2.9%,2.0%-7.4%and 0.3-5 mg/mL,respectively,while for HF-^(1)H qNMR,the intra-day RSDs,in⁃ter-day RSDs and LOQs were 0.40%-1.1%,1.5%-3.9%and 0.003-0.05 mg/mL,respective⁃ly.Both LF-^(1)H qNMR and HF-^(1)H qNMR were applied to the quantification of 167 seized ket⁃amine samples.The quantitative relative errors of LF-^(1)H qNMR and HF-^(1)H qNMR for ketamine and adulterants were all lower than 15%.The purity ranges of ketamine,dimethyl sulfone,sulfanil⁃amide,niacinamide,and phenacetin determined by LF-^(1)H qNMR were 13.5%-102.6%,1.1%-81.3%,2.6%-83.4%,1.8%-22.7%and 3.4%-43.8%,respectively,while those of ketamine,dimethyl sulfone,sulfanilamide,niacinamide and phenacetin determined by HF-^(1)H qNMR were 13.2%-99.7%,1.0%-78.4%,2.5%-75.9%,1.7%-21.3%and 3.0%-43.5%,respectively.Both LF-^(1)H qNMR and HF-^(1)H qNMR could realize the simultaneous quantitative analysis of ketamine and the adulterants without using reference materials.Although the precision and sensitivity of LF-^(1)H qNMR are slightly lower than those of HF-^(1)H qNMR,its simultaneous quantification ability toward multi-components in complex matrices is exciting.LF-^(1)H qNMR will be more widely used in forensic science laboratories in the future due to its low costs in instrument purchase and daily maintenance.

关 键 词：毒品 氯胺酮 掺杂物 定量分析 高场核磁共振 低场核磁共振 

分 类 号：O657.61[理学—分析化学] S859.81[理学—化学]