南方农业学报2026，Vol.57Issue(3)：659-672,14.DOI:10.3969/j.issn.2095-1191.2026.03.005
基于UPLC-MS/MS解析九制陈皮加工过程中生物碱的变化趋势
Alkaloid variation trend during the processing of nine-processed tangerine peel based on UPLC-MS/MS
摘要
Abstract
[Objective]To analyze the variation patterns of alkaloid compounds during the processing of nine-processed tangerine peel,which could provide theoretical basis for optimizing its processing procedures and quality con-trol.[Method]Citrus peels from four key processing stages of nine-processed tangerine peel,raw material(CP1),soa-king(CP2),pickling(CP3),and aging(CP4),were selected as experimental samples.Ultra-performance liquid chroma-tography coupled with tandem mass spectrometry(UPLC-MS/MS)was used in combination with principal component analysis(PCA),cluster analysis,and orthogonal partial least squares discriminant analysis(OPLS-DA)to investigate variation trend in alkaloid metabolites at the four key processing stages.Differential metabolites were identified through significance testing,fold change analysis,K-means cluster,and KEGG pathway annotation.[Result]A total of 33 alka-loids and their derivatives were identified across the four key processing stages of nine-processed tangerine peel.These in-cluded 10 indole alkaloids,3 quinoline alkaloids,each 2 of organic amines,pyridines,acridones,and phenethylamines,each 1 of quaternary ammonium compound,piperidine,pyrrole,and purine,and 8 alkaloid derivatives.Synephrine showed the highest relative content,followed by stachydrine.Based on the criteria of Fold Change≥1.5 or Fold Change≤0.67,together with variable importance in projection(VIP)≥1,30 significantly differential metabolites were screened,accounting for 90.9%of the total alkaloids.The comparisons of CP1 vs CP2,CP2 vs CP3,CP3 vs CP4,and CP1 vs CP4 contained 22,17,10,and 23 significantly differential metabolites respectively.During the overall proces-sing of nine-processed tangerine peel,the relative contents of alkaloids showed a general decreasing trend,with indole al-kaloids exhibiting the most pronounced decline,and the major changes mainly occurring during the soaking stage.The up-regulated differential metabolites included DL-2-aminoadipic acid,nicotine glucuronide,acetylcholine,and betaine,whereas the down-regulated differential metabolites were mainly indole alkaloids,such as 4-aminoindole,N-acetyl-5-hy-droxytryptamine,and methoxyindoleacetic acid.The main KEGG metabolic pathways annotated for the differential me-tabolites included tryptophan metabolism,biosynthesis of secondary metabolites,ABC transporters,as well as glycine,serine,and threonine metabolism.[Conclusion]During the processing of nine-processed tangerine peel,soaking is the key stage for the reduction and transformation of alkaloids contents.In practical production,soaking parameters,such as soaking time and temperature,can be optimized to balance the retention of major active components with the removal of bitter substances.Meanwhile,the contents of major active components,such as synephrine,and the transformation of indole compounds should be monitored.关键词
九制陈皮/生物碱/代谢组学/差异代谢物/超高效液相色谱串联质谱(UPLC-MS/MS)Key words
nine-processed tangerine peel/alkaloids/metabolomics/differential metabolites/ultra-performance li-quid chromatography coupled with tandem mass spectrometry(UPLC-MS/MS)分类
农业科技引用本文复制引用
陈楚,余元善,卜智斌,钟楚敏,郑慧珊,肖更生,傅曼琴..基于UPLC-MS/MS解析九制陈皮加工过程中生物碱的变化趋势[J].南方农业学报,2026,57(3):659-672,14.基金项目
广东省科技计划项目(2024A0505090019) （2024A0505090019）
澳门特别行政区科学技术发展基金项目(0076/2024/AGJ) Guangdong Science and Technology Plan Project(2024A0505090019) （0076/2024/AGJ）
Science and Technology Development Fund Project of Macao Special Administrative Region(0076/2024/AGJ) （0076/2024/AGJ）
