食品与发酵工业 >

2025 , Vol. 51 >Issue 16: 332 - 341

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.040602

分析与检测

N, O-双(三甲基硅烷)三氟乙酰胺硅烷化-气质联用法同时分析花椒风味和营养成分

  • 王群娣 ,
  • 韩冷 ,
  • 王旭婷 ,
  • 赵晨露 ,
  • 程玉娇 ,
  • 余波 ,
  • 邓明雪 ,
  • 张腾辉 ,
  • 李贵节
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  • 1(西南大学 柑桔研究所,重庆,400712)
    2(中国农业科学院柑桔研究中心,重庆,400712)
    3(国家柑桔工程技术研究中心,重庆,400712)
    4(农业农村部柑橘类果品质量安全控制重点实验室,重庆,400712)
    5(四川省丹橙现代果业有限公司,四川 眉山,620299)
    6(四川省丹棱县农业农村局,四川 眉山,620299)
    7(重庆市华测检测技术有限公司,重庆,400700)
第一作者:硕士研究生(程玉娇副研究员和李贵节副研究员为共同通信作者,E-mail:chengyujiao@cric.cn;liguijie@swu.edu.cn)

收稿日期: 2024-07-19

  修回日期: 2024-11-22

  网络出版日期: 2025-08-29

基金资助

重庆市自然科学基金项目(CSTB2023NSCQ-MSX0282);中央高校基本科研业务费专项资金项目(SWU-KR22050,SWU-KQ22057);西南大学国内合作项目(2023001206)

收起

Simultaneous analysis of flavor and nutritional components from Sichuan pepper using a N, O-bis (rimethylsilyl) trifluoroacetamide silylation-gas chromatography-mass spectrometry method

  • WANG Qundi ,
  • HAN Leng ,
  • WANG Xuting ,
  • ZHAO Chenlu ,
  • CHENG Yujiao ,
  • YU Bo ,
  • DENG Mingxue ,
  • ZHANG Tenghui ,
  • LI Guijie
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  • 1(Citrus Research Institute, Southwest University, Chongqing 400712, China)
    2(Citrus Research Center, Chinese Academy of Agricultural Sciences, Chongqing 400712, China)
    3(National Citrus Engineering Research Center, Chongqing 400712, China)
    4(Key Laboratory of Quality and Safety Control of Citrus Fruits, Ministry of Agriculture and Rural Affairs, Chongqing 400712, China)
    5(Sichuan Dancheng Modern Fruit Industry Co.Ltd., Meishan 620299, China)
    6(Danling County Agriculture and Rural Bureau, Meishan 620299, China)
    7(Chongqing Centre Testing International Group Co.Ltd., Chongqing 400700, China)

Received date: 2024-07-19

  Revised date: 2024-11-22

  Online published: 2025-08-29

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摘要

花椒是我国重要调味料之一,含有花椒酰胺、挥发油、脂肪酸和维生素等成分,有很高的经济价值。为全面快速地分析检测花椒中主要的风味和营养物质,该研究以N,O-双(三甲基硅烷)三氟乙酰胺[N,O-bis(rimethylsilyl)trifluoroacetamide,BSTFA]为硅烷化试剂,开发柱前衍生化反应结合GC-MS联用测定方法,通过选择硅烷化反应产物特征离子等手段分析鉴定花椒成分,并采用感官评价、最小二乘回归分析和相关性分析进一步探究花椒感官属性与风味化合物之间的关系。结果显示,在干花椒、花椒油和花椒精油样品中,该方法共鉴定出五大类主要成分,包括花椒酰胺3种、挥发油17种、脂肪酸6种、维生素1种及可溶性糖3种。衍生后各物质分离效果良好,能够实现准确定性和定量分析。3种样品中,花椒精油所含花椒酰胺最高,其羟基-β-山椒素含量为54.77 μg/g;其芳樟醇含量为1 388.13 μg/g,也远高于其他样品。花椒精油的感官品评得分最高,干花椒和花椒油评分依次降低。最小二乘回归和相关性分析表明评分结果与关键风味物质定量结果基本相符。该方法具有快速高效和应用广的特点,可同时测定原样中挥发和不易挥发物质,从而大幅提高花椒及制品中主要风味和营养物质的检测效率。

关键词： 花椒; 硅烷衍生化; 气质联用; 花椒酰胺; 挥发油; 脂肪酸; 维生素

本文引用格式

王群娣 , 韩冷 , 王旭婷 , 赵晨露 , 程玉娇 , 余波 , 邓明雪 , 张腾辉 , 李贵节 . N, O-双(三甲基硅烷)三氟乙酰胺硅烷化-气质联用法同时分析花椒风味和营养成分[J]. 食品与发酵工业, 2025 , 51(16) : 332 -341 . DOI: 10.13995/j.cnki.11-1802/ts.040602

Abstract

Sichuan pepper is one of the important seasonings in China, containing components such as zanthoxylamide, volatile oil, fatty acids, and vitamins, and it has significant economic value.To comprehensively and rapidly analyze and detect the main flavor and nutritional substances in Sichuan pepper, this study developed a method using N, O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) as the silylation reagent, combining pre-column derivatization with gas chromatography-mass spectrometry (GC-MS) analysis.The components of Sichuan pepper were analyzed and identified through the selection of characteristic ions of silylation reaction products.Additionally, sensory evaluation, partial least squares regression analysis, and correlation analysis were employed to further investigate the relationship between the sensory attributes and flavor compounds of Sichuan pepper.Results showed that in dried Sichuan pepper, Sichuan pepper oil, and Sichuan pepper essential oil samples, a total of five major categories of components were identified by this method, including 3 zanthoxylamides, 17 volatile oil compounds, 6 fatty acids, 1 vitamin, and 3 soluble sugars.The derivatized substances exhibited good separation efficiency, enabling accurate qualitative and quantitative analysis.Among the three samples, the essential oil had the highest content of zanthoxylamides, with a hydroxy-β-sanshool content of 54.77 μg/g, its linalool content, 1 388.13 μg/g, was also significantly higher than other samples.The sensory evaluation score of the essential oil was the highest, followed by dried Sichuan pepper and Sichuan pepper oil.Partial least squares regression and correlation analysis indicated that the sensory evaluation results were generally consistent with the quantitative results of key flavor compounds.This method is characterized by its rapidity, efficiency, and broad applicability, allowing simultaneous determination of both volatile and non-volatile substances in the original samples, thereby significantly improving the detection efficiency of major flavor and nutritional substances in Sichuan pepper and its products.

Key words： Zanthoxylum; silylation; GC-MS; zanthoxylamide; volatile oil; fatty acid; vitamin

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