GC-Q/TOF MS融合多手段非靶向分析烟草提取物成分  

Multiple techniques in combination with GC-Q/TOF MS for non-targeted analysis of tobacco extract components

作　　者：沈海峰 张华[2] 王晨辉[2] 董卉林 任家乐 朱怀远[2] 廖惠云[2] 迟波[1] SHEN Haifeng;ZHANG Hua;WANG Chenhui;DONG Huilin;REN Jiale;ZHU Huaiyuan;LIAO Huiyun;CHI Bo(College of Food Science and Light Industry,Nanjing Tech University,Nanjing 211816,China;China Tobacco Jiangsu Industrial Co.,Ltd.,Nanjing 210019,China)

机构地区：[1]南京工业大学食品与轻工学院,南京市211816 [2]江苏中烟工业有限责任公司,南京市210019

出　　处：《烟草科技》2024年第9期1-15,共15页Tobacco Science & Technology

基　　金：中国烟草总公司科技项目“废次烟叶的渗透汽化提取分离耦合技术开发及规模化应用”(110202202024);江苏中烟工业有限责任公司对外合作科技创新项目“复杂基质体系中烟草提取物组分解析及应用研究”(H202228);江苏中烟工业有限责任公司科技创新项目“高分辨质谱分析常用天然植物提取物及其在仿香中的应用”(202410)。

摘　　要：为完善复杂基质样品非靶向定性分析结果,采用解卷积提取总离子流色谱图(TIC),融合谱库检索、保留指数(RI)、碎片离子精确质量数以及分子结构关联等多种手段,建立了使用气相色谱-四极杆飞行时间串联质谱(GC-Q/TOF MS)技术分析烟草提取物中挥发性、半挥发性化学成分的方法。结果表明:①在标准EI电离模式下采集样品,通过NIST等谱库检索和RI对比,设置合适的过滤条件,初步鉴定出97种化合物;②对于匹配度符合要求但RI偏离范围的组分,结合精确质量数辅助鉴别,再定性出52种化合物;③对于色谱峰响应高但匹配度不好的组分,进一步采用GC-Q/TOF MS低能量电离模式,通过确定其分子离子峰和二级质谱推断分子式,并结合Chemspider在线方式定性出NIST谱库外化合物2种,分别为3-羟基-7,8-二脱氢-β-紫罗兰醇和(3R,4R)-3-(2-苯乙基)-1-十二烯-3,4-二醇。融合多种分析手段,从烟草提取物中共鉴定出包括烟碱以及醇类、酯类、醛类、酮类、酸类、烷烃类、烯烃类、酚类、胺类、醚类和其他类化合物等共151种。该研究可为复杂基质提取物中挥发性、半挥发性组分的非靶向分析提供新思路,尤其是GC-Q/TOF MS的精确质量数和可变能量电离模式结合二级质谱联用分子结构关联丰富了化合物的鉴定手段。To improve the results of non-targeted qualitative analysis of complex matrix samples,a combinatory strategy for analyzing volatile and semi-volatile chemical components in tobacco extracts with gas chromatography-quadrupole time-of-flight tandem mass spectrometry(GC-Q/TOF MS)was developed.The method adopted techniques such as deconvolutional extraction of total ion flow chromatography(TIC),fusion library retrieval,retention index(RI),precise mass number of fragment ions,and molecular structure correlation.The results showed that:1)Samples collected under the standard EI ionization mode displayed 97 compounds that could be preliminarily identified through NIST library retrieval and RI comparison under appropriate filtering conditions.2)For those components that met the matching requirements but deviated from the RI range,52 compounds were qualitatively identified by combining with precise mass number assistance.3)For those components with higher chromatographic peak responses but poorer matching degrees,the GC-Q/TOF MS low-energy ionization mode was further used to determine their molecular ion peaks and secondary mass spectrometry to infer their molecular formula.Combined with the Chemspider,two compounds outside the NIST library were online qualitatively identified as 3-hydroxy-7,8-didehydro-β-ionol and(3R,4R)-3-(2-phenylethyl)-1-dodecene-3,4-diol.By integrating these analytical methods,a total of 151 compounds including nicotine,alcohols,esters,aldehydes,ketones,acids,alkanes,olefins,phenols,amines,ethers,and other compounds were identified from the tobacco extract.This study provides an improved approach for the non-targeted analysis of volatile and semi-volatile components in complex matrix extracts,especially combining the precise mass number and variable energy ionization mode of GC-Q/TOF MS with secondary mass spectrometry molecular structure correlation enriches the numbers and accuracies of the compounds identified.

关 键 词：烟草 提取物 复杂基质 气相色谱-四极杆飞行时间串联质谱 可变能量电离 非靶向分析 成分鉴定 

分 类 号：TS411.1[农业科学—烟草工业]