固相微萃取-气质联用技术分析全蝎氧化酸败过程中挥发性成分的变化  

Changes of volatile components during oxidative rancidity of Scorpion analyzed by SPME-GC-MS

作　　者：左凯 何旭峰 黄小兰 阳文武 伍蓉 曹纬国[1,4] ZUO Kai;HE Xu-feng;HUANG Xiao-lan;Yang Wen-wu;WU Rong;CAO Wei-guo(College of Traditional Chinese Medicine,Chongqing University of Medical Sciences,Chongqing 400016,China;Chongqing Institute for Food and Drug Control,Chongqing 404047,China;Chongqing Key Laboratory of Development and Utilization of Genuine Medicinal Materials in Three Gorges Reservoir Area,Chongqing 404120,China;Chongqing University of Chinese Medicine,College of Chinese Materia Medica,Chongqing 402760,China)

机构地区：[1]重庆医科大学中医药学院,重庆400016 [2]重庆市食品药品检验检测研究院,重庆404047 [3]三峡库区道地药材开发利用重庆市重点实验室,重庆404120 [4]重庆中医药学院中药学院,重庆402760

出　　处：《药物分析杂志》2024年第11期1958-1966,共9页Chinese Journal of Pharmaceutical Analysis

基　　金：国家药品监督管理局药品监管科学体系建设重点项目(RS2024Z006);重庆市药品监督管理局、重庆市科技局联合项目(渝药监[2023]24号);三峡库区道地药材开发利用重庆市重点实验室项目(Sys20210020)。

摘　　要：目的:分析全蝎氧化酸败过程中挥发性成分的变化,鉴定引起全蝎哈喇味的主要成分。方法:对全蝎样品进行50 d的加速氧化实验,从0 d开始,每隔10 d进行样品感官评价,同时利用固相微萃取-气质联用技术检测其挥发性成分,共得6组数据。将所得挥发性成分进行计算机检索,结果与NIST20数据库匹配,鉴定其化学结构,同时以2-辛醇为内标,计算挥发性成分的相对含量,结合主成分分析和聚类分析筛选出全蝎哈喇味的主要成分。结果:从全蝎中共检出醛类、酸类、呋喃类等挥发性成分51个,其中43个为6组数据所共有。不同氧化阶段全蝎挥发性成分含量存在明显差异,醛类物质含量最高,均值为101.33 mg·kg^(-1),占比54.45%,其次是酸类物质,均值为52.01 mg·kg^(-1),占比27.95%。随着氧化时间的延长,全蝎出现哈喇味,当氧化50 d后,出现重度哈喇味;同时各类别挥发性成分含量均呈上升趋势,其中庚醛、壬醛、正辛醛、2-丁基-2-辛烯醛、4-氧代-2-壬烯醛、己酸、2-正戊基呋喃含量增幅明显,增长倍数为4倍~44倍。通过主成分分析,提取出3个特征值>1的主成分,其中主成分1的特征值为40.451,特征值贡献率为79.32%,主要影响因子为醛类、酸类、呋喃类物质。聚类分析将6组样品分为4类,与感官评价结果一致。结论:庚醛、壬醛、正辛醛、2-丁基-2-辛烯醛、4-氧代-2-壬烯醛、己酸、2-正戊基呋喃7个挥发性成分是全蝎产生哈喇味的主要物质;本试验为开发简捷、精准监测全蝎氧化酸败过程提供新技术新方法,同时为全蝎质量标准的提升提供研究基础。Objective:To analyze the variation of volatile components during oxidative rancidity of Scorpion,and identify the main components resulting in the rancid flavor of Scorpion.Methods:Scorpion samples were subjected to accelerated oxidation experiment for 50 d,starting from 0 d,and sensory evaluation of the sample was performed every 10 d.At the same time,the volatile components were detected by solid phase microextraction GC-MS(SPME-GC-MS).Six groups of data were obtained.The volatile components obtained were searched by computer,and the results were matched with the NIST 20 database to determine the chemical structure of that.Meanwhile,the relative content of volatile components was calculated by using 2-octanol as internal standard,and the main components of Scorpion's rancid flavor were screened out through principal component analysis and cluster analysis.Results:A total of 51 volatile components such as aldehydes,acids and furans were detected,of which 43 were common to six groups of data.There were significant differences in the content of volatile components of Scorpions in different oxidation time periods,with aldehydes being the highest,with an average content of 101.33 mg·kg^(-1),accounting for 54.45%,followed by acids,with an average content of 52.01 mg·kg^(-1),accounting for 27.95%.With the prolongation of the oxidation time,the Scorpion appeared to have a rancid flavor,when oxidized for 50 d,a heavy rancid flavor appeared;at the same time,the content of volatile components of all categories showed an increasing trend,among which the content of heptanal,nonanal,n-octanal,2-butyl-2-octenal,4-oxo-2-nonenal,hexanoic acid and 2-n-pentylfuran increased significantly,with an increase of multiples of 4 times to 44 times.Through principal component analysis,three principal components were screened out with eigenvalues above 1 value,among which the eigenvalue of principal component 1 was 40.451,and the contribution rate of that reached a 79.32%,the main influencing factors included aldehydes,acids and furans.S

关 键 词：全蝎 氧化酸败 挥发性成分 哈喇味 固相微萃取-气相色谱串联质谱 加速氧化试验 主成分分析 聚类分析 

分 类 号：R917[医药卫生—药物分析学]