Food and Fermentation Industries >

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

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

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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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

Cite this article

WANG Qundi , HAN Leng , WANG Xuting , ZHAO Chenlu , CHENG Yujiao , YU Bo , DENG Mingxue , ZHANG Tenghui , LI Guijie . Simultaneous analysis of flavor and nutritional components from Sichuan pepper using a N, O-bis (rimethylsilyl) trifluoroacetamide silylation-gas chromatography-mass spectrometry method[J]. Food and Fermentation Industries, 2025 , 51(16) : 332 -341 . DOI: 10.13995/j.cnki.11-1802/ts.040602

References

[1] LIANG W Y, YANG H Y, LEI H X, et al.Phytochemistry and health functions of Zanthoxylum bungeanum Maxim and Zanthoxylum schinifolium Sieb.et Zucc as pharma-foods:A systematic review[J].Trends in Food Science & Technology, 2024, 143:104225.
[2] 叶倩女, 石晓峰, 杨军丽.花椒属植物中酰胺类成分的结构与功能研究进展[J].中国中药杂志, 2023, 48(9):2406-2418.
YE Q N, SHI X F, YANG J L.Research advance on the structure and function of amides in Zanthoxylum plants[J].China Journal of Traditional Chinese Materia Medica, 2023, 48(9):2406-2418.
[3] 阚建全, 陈科伟, 任廷远, 等.花椒麻味物质的生理作用研究进展[J].食品科学技术学报, 2018, 36(1):11-17;44.
KAN J Q, CHEN K W, REN T Y, et al.Review on physiological function of alkylamide compounds from Zanthoxylum bungeanum[J].Journal of Food Science and Technology, 2018, 36(1):11-17;44.
[4] CHRUMA J J, CULLEN D J, BOWMAN L, et al.Polyunsaturated fatty acid amides from the Zanthoxylum genus-from culinary curiosities to probes for chemical biology[J].Natural Product Reports, 2018, 35(1):54-74.
[5] 高夏洁, 钟葵, 赵镭, 等.不同产区花椒油的椒麻感官特性及物质组成[J].食品科学, 2022, 43(8):281-287.
GAO X J, ZHONG K, ZHAO L, et al.Sensory numb taste characteristics and numb taste-active components of pepper oil produced in different areas of China[J].Food Science, 2022, 43(8):281-287.
[6] NI R J, YAN H Y, TIAN H L, et al.Characterization of key odorants in fried red and green huajiao (Zanthoxylum bungeanum maxim.and Zanthoxylum schinifolium sieb.et Zucc.) oils[J].Food Chemistry, 2022, 377:131984.
[7] ZHAO C, HAN M, TU T, et al.Comparative analysis of fatty acids, volatile and non-volatile components in red huajiao (Zanthoxylum bungeanum maxim.) and green huajiao (Zanthoxylum armatum DC.) using GC-MS, UPLC-LTQ-Orbitrap-MS/MS and HPLC-DAD[J].Industrial Crops and Products, 2023, 204:117371.
[8] SUN J, SUN B G, REN F Z, et al.Characterization of key odorants in Hanyuan and Hancheng fried pepper (Zanthoxylum bungeanum) oil[J].Journal of Agricultural and Food Chemistry, 2020, 68(23):6403-6411.
[9] 杨森, 何晗, 易达, 等.川产竹叶花椒挥发油中12种挥发性成分的测定与比较[J].食品与发酵工业, 2022, 48(8):270-275.
YANG S, HE H, YI D, et al Determination and comparison of 12 volatile components in volatile oil from Zanthoxylum armatum DC[J].Food and Fermentation Industries, 2022, 48(8):270-275.
[10] HOU L X, LIU Y L, WEI A Z.Geographical variations in the fatty acids of Zanthoxylum seed oils:A chemometric classification based on the random forest algorithm[J].Industrial Crops and Products, 2019, 134:146-153.
[11] MA Y, TIAN J Y, WANG X N, et al.Fatty acid profiling and chemometric analyses for Zanthoxylum pericarps from different geographic origin and genotype[J].Foods, 2020, 9(11):1676.
[12] 王俊贤, 喻阳华, 蓝家程, 等.顶坛花椒果实品质及随海拔的变异规律研究[J].核农学报, 2023, 37(9):1884-1893.
WANG J X, YU Y H, LAN J C, et al.Study on Fruit quality of Zanthoxyhum planispiunum var.dingtanensis and its variation with altitude[J].Journal of Nuclear Agricultural Sciences, 2023, 37(9):1884-1893.
[13] 马伟, 钟慈平, 何成军, 等.花椒及花椒制品中羟基-α-山椒素检测方法[J].食品工业, 2022, 43(9):65-70.
MA W, ZHONG C P, HE C J, et al.The determination of Hydroxyl-a-santhoxylin in Zanthoxylum and its products[J].Food industry, 2022, 43(9):65-70.
[14] 程玉波, 魏浩华, 曾钦朦, 等.贵州不同品种花椒麻味物质的测试分析[J].食品工业, 2022, 43(1):219-223.
CHENG Y B, WEI H H, ZENG Q M, et al.Test and analysis of hemp substance from different varieties of Zanthoxylum schinifolium in Guizhou[J].The Food Industry, 2022, 43(1):219-223.
[15] LIU Y P, LI Q R, YANG W X, et al.Characterization of the potent odorants in Zanthoxylum armatum DC Prodr.pericarp oil by application of gas chromatography-mass spectrometry-olfactometry and odor activity value[J].Food Chemistry, 2020, 319:126564.
[16] KHAKIMOV B, MOTAWIA M S, BAK S, et al.The use of trimethylsilyl cyanide derivatization for robust and broad-spectrum high-throughput gas chromatography-mass spectrometry based metabolomics[J].Analytical and Bioanalytical Chemistry, 2013, 405(28):9193-9205.
[17] HALKET J M, ZAIKIN V G.Derivatization in mass spectrometry:1.silylation[J].European Journal of Mass Spectrometry, 2003, 9(1):1-21.
[18] THI H T, LE B A, LE H N T, et al.Screening of fatty acids, saccharides, and phytochemicals in Jatropha curcas seed kernel as their trimethylsilyl derivatives using gas chromatography/mass spectrometry[J].Journal of Chromatography B-Analytical Technologies in the Biomedical and Life Sciences, 2018, 1102-1103:66-73.
[19] YANG G S, IV E C, WANG H W.Flavor lexicon development (in English and Chinese) and descriptive analysis of Sichuan pepper[J].Journal of Sensory Studies, 2021, 36(2):e12636.
[20] ZHAO M, LI T, YANG F, et al.Characterization of key aroma-active compounds in Hanyuan Zanthoxylum bungeanum by GC-O-MS and switchable GC×GC-O-MS[J].Food Chemistry, 2022, 385:132659.
[21] COCITO C, DELFINI C.Simultaneous determination by GC of free and combined fatty acids and sterols in grape musts and yeasts as silanized compounds[J].Food Chemistry, 1994, 50(3):297-305.
[22] ZHANG S M, WANG H B, ZHU M J.A sensitive GC/MS detection method for analyzing microbial metabolites short chain fatty acids in fecal and serum samples[J].Talanta, 2019, 196:249-254.
[23] YAN B, JIYE A, WANG G J, et al.Metabolomic investigation into variation of endogenous metabolites in professional athletes subject to strength-endurance training[J].Journal of Applied Physiology, 2009, 106(2):531-538.
[24] 杨静, 赵镭, 史波林, 等.青花椒香气快速气相电子鼻响应特征及GC-MS物质基础分析[J].食品科学, 2015, 36(22):69-74.
YANG J, ZHAO L, SHI B L, et al.Aroma response characteristic analysis with fast gas phase electronic nose and volatile components analysis with GC-MS of green prickly ash[J].Food Science, 2015, 36 (22):69-74.
[25] GAO L, SHI B L, ZHAO L, et al.Aroma characteristics of green Huajiao in Sichuan and Chongqing area using sensory analysis combined with GC-MS[J].Foods, 2024, 13(6):836.
[26] 董天宇, 齐楠, 刘芮嘉, 等.青花椒与红花椒关键风味物质的对比分析[J].精细化工, 2023, 40(4):869-877.
DONG T Y, QI N, LIU R J, et al.Comparative analysis of key flavor substances of green and red pepper[J].Fine Chemicals, 2023, 40(4):869-877.
[27] 高露, 赵镭, 史波林, 等.气相色谱-质谱联用结合气味活度值分析红花椒油的关键香气物质特征[J].食品与发酵工业, 2023, 49(22):295-301.
GAO L, ZHAO L, SHI B L, et al.GC-MS combined with odor activity value to analyze key aroma substance characteristics of red Chinese pepper oil[J].Food and Fermentation Industries, 2023, 49(22):295-301.
[28] 陈茜, 陶兴宝, 黄永亮, 等.花椒香气研究进展[J].中国调味品, 2018, 43(1):189-194.
CHEN Q, TAO X B, HUANG Y L, et al Research progress on the aroma of Chinese prickly ash[J].Chinese Seasoning, 2018, 43(1):189-194.
[29] 李开, 张嘉铭, 郝瀚, 等.两种冷榨工艺红橘精油挥发性成分对比分析[J].食品工业科技, 2024, 45(19):286-295.
LI K, ZHANG J M, HAO H, et al.Comparative analysis of volatile components in red orange essential oil extracted by two cold pressing processes[J].Science and Technology of Food Industry, 2024, 45(19):286-295.
[30] YANG X G.Aroma constituents and alkylamides of red and green huajiao (Zanthoxylum bungeanum and Zanthoxylum schinifolium)[J].Journal of Agricultural and Food Chemistry, 2008, 56(5):1689-1696.
[31] FENG X Y, HUANG P M, DUAN P, et al.Dynamic Zanthoxylum pungency characteristics and their correlation with sanshool composition and chemical structure[J].Food Chemistry, 2023, 407:135138.
[32] DELMAS P, COSTE B.SnapShot:Orofacial sensation[J].Cell, 2020, 183(1):284-284.
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