色谱2025，Vol.43Issue(2)：164-176,13.DOI:10.3724/SP.J.1123.2024.02008
在线固相萃取-液相色谱-线性离子阱质谱法同时检测尿液和血液中51种吲唑类合成大麻素
Simultaneous determination of 51 indazole-type synthetic cannabinoids in urine and blood by online solid-phase extraction-liquid chromatography-linear ion trap mass spectrometry
摘要
Abstract
To evade legal controls,new psychoactive substances(NPS),which have been de-signed as substitutes for traditional and synthetic drugs,are gradually dominating the drug market.Synthetic cannabinoids(SCs),which account for the majority of NPS,are rapidly be-ing derivatized;consequently,controlling increasing abuse by merely listing individual com-pounds is difficult.Therefore,China has included the entire SC category of SCs listed as legal controlled substances since July 1,2021.However,new SCs obtained through structural modifi-cation are still appearing and pose significant analytical challenges for forensic laboratories.Therefore,an efficient,green,and automated detection method is urgently required to provide technical support for the accurate screening actual samples.Meanwhile,the number of in-dazole-type SCs has increased sharply since 2013,which is ascribable to their stronger psycho-active effects.Indeed,forensic laboratories mainly analyze this key SC subclass.Therefore,in this study,we developed a new method for analyzing 51 indazole-type SCs in human urine and blood,which involves online solid-phase extraction(online SPE)as the preprocessing technol-ogy,with analysis performed using liquid chromatography-linear ion trap mass spectrometry.Deproteinization was achieved by adding acetonitrile,with dilution performed using 10 mmol/L ammonium acetate solution(pH 4.8)containing 0.1％formic acid.Samples were then analyzed directly using acetonitrile-10 mmol/L ammonium acetate aqueous solution(containing 0.1％formic acid)as the mobile phase.The mass-to-charge ratios of protonated molecular ions([M+H]+)in the mass spectra acquired in full-scan mode,and the retention times in the chromato-grams of the analytes were selected with the aim of monitoring the MS2 ions of the various com-pounds.Characteristic fragment ions of the various SC structures were summarized,with five groups of isomers,each containing ten compounds,successfully distinguished using multistage mass spectrometry and their retention times.Multistage MS was used to qualitatively screen 51 indazole-type SCs,which were then quantitatively analyzed using MS2 ion pairs(as quantitative ion pairs).The analytes exhibited limits of detection(LODs)of 0.02-1 ng/mL,with limits of quantification(LOQs)of 0.04-4 and 0.1-4 ng/mL in urine and blood,respectively.Linear fit-ting(weighting factor 1/x)revealed good linearity for each analyte within its respective linear range,with correlation coefficients(R2)greater than 0.99 in both urine and blood.The validity of the analytical method was tested by determining precision and spiked recovery values(n=6).Recoveries of 83.47％-116.95％were obtained at LOQ levels,with precisions of 2.29％-13.40％.In addition,recoveries of 86.63％-113.38％and precisions of 0.58％-13.79％were ob-tained at low,medium,and high levels.The method described herein is not only easy to oper-ate but also can be automated.Indeed,high-throughput sample analysis was achieved when sample extraction,enrichment,and analysis were performed in dynamic mode through valve switching.Meanwhile,the method exhibited good sensitivity and is applicable to a wider range of compounds than those previously reported;it also provides a scientific basis and technical support for the rapid screening and quantitative analysis of SCs in actual relevant cases.关键词
合成大麻素/吲唑类/尿液/血液/在线固相萃取/液相色谱-线性离子阱质谱Key words
synthetic cannabinoids(SCs)/indazole-type/urine/blood/online solid-phase ex-traction(online SPE)/liquid chromatography-linear ion trap-mass spectrometry(LC-LIT-MS)分类
化学化工引用本文复制引用
罗轩,张珺,朱定姬,黄克建,杨宁,刘晓锋,罗秋莲..在线固相萃取-液相色谱-线性离子阱质谱法同时检测尿液和血液中51种吲唑类合成大麻素[J].色谱,2025,43(2):164-176,13.基金项目
广西科技计划项目(桂科AD19259004).Guangxi Science and Technology Project(No.Guike AD19259004). （桂科AD19259004）
