高效液相色谱-四极杆/飞行时间质谱的源内裂解-多级质谱法解析干燥恰特草中卡西酮类生物碱成分

扫码查看

原文链接

万方数据
维普

中文摘要：本研究基于高效液相色谱-四极杆/飞行时间质谱(HPLC-Q-TOF MS)的源内裂解-多级质谱法,发现并解析了恰特草中未知卡西酮类生物碱成分.将恰特草粉碎后,采用0.05 mol/L HCl水溶液提取,二氯甲烷、NaOH 水溶液净化,ZORBAX Eclipse Plus Phenyl-Hexyl 色谱柱(3.0 mm × 100 mm × 1.8 μm)以0.1％甲酸水(A)-乙腈(B)为流动相进行梯度洗脱.在一级质谱全扫描模式下,通过卡西酮类生物碱的源内裂解特征实现未知卡西酮类生物碱成分的筛查;在目标离子采集模式下,基于未知卡西酮类生物碱成分的多级质谱裂解规律推测其分子结构.结果表明,该方法可实现恰特草中未知生物碱成分的筛查和解析,共识别出甲卡西酮、乙卡西酮和2-氨基-1-苯基-1-丁酮等3种卡西酮类生物碱成分,并采用标准物质对甲卡西酮和乙卡西酮进行确证,但由于缺乏相应的标准物质,2-氨基-1-苯基-1-丁酮有待进一步确证.本工作为恰特草中精神活性成分的进一步研究提供指引,为其他领域未知化合物的解析提供参考.

外文标题：Analysis of Cathinone Alkaloids in Khat by HPLC-Q-TOF In-source Fragmentation Multistage Mass Spectrometry

外文摘要：Khat is a kind of common drug plant.Many experiments have shown that the content of cathinone norpseudoephedrine and norephedrine in some varieties of Khat are similar.However,some studies showed that there are differences in the intensity of psychoactivity between these varieties.Therefore,it is speculated that other substances in Khat may affect the psychoactive strength of Khat.But currently there are some difficulties in non-targeted screening of unknown compounds without mass spectrometry database information and standard solutions.In this paper,the unknown cathinone alkaloids in Khat were discovered and resolved by HPLC-Q-TOF MS in-source fragmen-tation multistage mass spectrometry.The separation was carried out on a ZORBAX Eclipse Plus Phenyl-Hexyl column(3.0 mm× 100 mm× 1.8 μm)with a gradient elution using 0.1％formic acid in water(A)-acetonitrile(B)as the mobile phase.The mobile phase flow rate was 0.3 mL/min,and the column temperature was 30 ℃.The screening of unknown cathinone alkaloid components was realized by the in-source cleavage char-acteristics of cathinone alkaloids in single-stage mass spectrometry under full-scan mode using an ESI ion source,and then the molecular structures of the unknown cathinone alkaloid components were deduced from the multi-stage MS cleavage patterns of the unknown cathinone alkaloid components in the target ion acquisition mode.The results showed that this method can effectively realize the screening and resolution of the unknown alkaloid components in Khat.A total of three cathinone alkaloid components,including methcathinone,ethcathinone and 2-amino-1-phenyl-1-butanone,were identi-fied in Khat.Methcathinone and ethcathinone were corroborated using standard substances,and 2-amino-1-phenyl-1-butanone needs to be further corroborated due to the lack of corresponding standard substances.The work provides a guideline for the further study of the psychoactive components in Khat,and a reference for the analysis of unknown compounds in other fields.

外文关键词：

high performance liquid chromatography-quadrupole-time of flight mass spectrometry(HPLC-Q-TOF MS)in-source fragmentation multistage mass spectrome-tryKhatcathinone alkaloidsanalysis of unknown compounds

作者：

史洪飞、徐伯芃、权养科、徐成鑫、周修齐

展开 >

作者单位：

南京警察学院刑事科学技术学院,江苏南京 210023

公安部鉴定中心,北京 100038

关键词：

高效液相色谱-四极杆/飞行时间质谱(HPLC-Q-TOF MS) 源内裂解-多级质谱法恰特草卡西酮类生物碱未知物解析

基金：

刑事检验四川省高等学校重点实验室开放基金国家级大学生创新重点项目(2023)

项目编号：

2023YB05202312213025Z

出版年：

2024

DOI：

10.7538/zpxb.2023.0065

质谱学报

北京中科科仪技术发展有限责任公司中国物理学会质谱分会

质谱学报

CSTPCD北大核心EI

影响因子：1.046

ISSN：1004-2997

年,卷(期)：2024.45(2)

参考文献量40