基于UPLC-Q-TOF-MS技术的益智种子和果皮成分分析  

UPLC-Q-TOF-MS Based Analysis of Chemical Constituents of Seeds and Peels of Alpinia oxyphylla

作　　者：王茂媛[1,3,4] 王祝年 王清隆[1,2] 羊青 张旻[5] 晏小霞 WANG Maoyuan;WANG Zhunian;WANG Qinglong;YANG Qing;ZHANG Min;YAN Xiaoxia(Tropical Crops Genetic Resources Institute,Chinese Academy of Tropical Agricultural Sciences,Haikou,Hainan 571101,China;National Tropical Plants Germplasm Resource Center,Haikou,Hainan 571101,China;Tropical Wild Plant Gene Resource,Ministry of Agriculture&Rural Affairs,Danzhou,Hainan 571737,China;Hainan Provincial Engineering Research Center for Tropical Medicinal Plant,Danzhou,Hainan 571737,China;Key Laboratoory of Southem Subtropical Plant Diversity,Shenzhen Fairy Lake Botanical Garden,Shenzhen&Chinese Academy of Sciences,Shenzhen,Guangdong 518004)

机构地区：[1]中国热带农业科学院热带作物品种资源研究所,海南海口571101 [2]国家热带植物种质资源库,海南海口571101 [3]农业农村部热带农业野生植物基因资源鉴定评价中心,海南儋州571737 [4]海南省热带药用植物工程研究中心,海南儋州571737 [5]深圳市中国科学院仙湖植物园/深圳市南亚热带植物多样性重点实验室,广东深圳518004

出　　处：《热带作物学报》2022年第5期1064-1075,共12页Chinese Journal of Tropical Crops

基　　金：中央级公益性科研院所基本科研业务费专项(No.1630032021021);海南省自然科学基金项目(No.820QN344,No.320QN342)。

摘　　要：基于UPLC-Q-TOF-MS技术对益智种子和果皮乙醇提取物的非挥发性成分进行分析。采用回流提取法制备供试样品,采用超高效液相色谱仪分离益智种子和果皮乙醇提取物化学成分,以Waters ACQUITY UPLC HSS T3(100 mm×2.1 mm,1.8μm)色谱柱为分析柱,0.1%甲酸水溶液–0.01%甲酸乙腈溶液为流动相进行梯度洗脱,流速0.3mL/min,质谱采用电喷雾离子源(ESI),四极杆-飞行时间质谱采集其一级和二级高分辨质谱数据,并用Masslynx软件对原始质谱数据进行分子特征提取,结合文献报道信息,综合分子相应结构特征、精确相对分子质量和质谱裂解规律,对化合物结构进行识别鉴定。从益智种子和果皮乙醇提取物中分别鉴定32个和50个非挥发性成分,包括黄酮类、酚酸类、糖类、脂肪酸类和萜类化合物等5类成分,其中有58个化合物为首次从益智中分离得到;益智种子的主要成分为酚酸类(11个)化合物,也是益智种子的代表性成分,占总鉴定结构化合物总数的三分之一,而益智果皮中的酚酸类成分较少,仅鉴定得到6个酚酸类化合物;益智果皮主要成分为黄酮类(19个)化合物,占总鉴定结构的化合物总数近三分之一,且种类丰富,而种子中仅鉴定得到1个黄酮类化合物;二者中共有成分仅4个,分别是单糖类化合物D-gluconic acid、D-glucopyranuronic acid,二糖类化合物sucrose和黄酮类化合物chysin。结果表明,益智种子非挥发性化学物质较少,而益智果皮中含有的化学物质种类较多;益智种子和果皮的化学成分差异较大:益智种子主要成分为酚酸类活性物质,益智果皮则以黄酮和萜类成分为主,在综合利用和质量控制上应区别对待使用。The purpose of this paper was to analyze and identify the nonvolatile components of the ethanol extract in the seeds and peels of Alpinia oxyphylla.The extracts were prepared by the refluxing methods,high-resolution mass spectrometric data of the extract were collected by the ultra performance liquid chromatography coupled with quadrupole-time of flight-tandem mass spectrometry(UPLC-Q-TOF-MS).The main components in the extracts were separated by the gradient elution method with waters ACQUITY UPLC HSS T3(100 mm×2.1 mm,1.8μm),the mobile phase consisted of 0.1%formic acid and 0.01%formic acid acetonitrile,with the flow rate of 0.3 mL/min.Mass spectrometry was applied for the qualitative analysis with ESI ion source.Through molecular feature extraction(MFE),Masslynx software was then used to process the original MS data.Furthermore,the structures of the compounds were speculated according to the MS fragmentation patterns and confirmed by comparison with reference standards.Thirty-two and fifty compounds were identified from the seeds and peels respectively,including flavonoids,phenolic acids,saccharides,fatty acids and terpenes.58 compounds were isolated from the plant for the first time.The main constituents of the seeds were phenolic acids(11 compounds),which were representative constituents of the seeds,accounting for one third of the total identified structural compounds of the seeds.On the contrary,there were few phenolic acids in the peels.The main constituents of the peels were flavonoids(19 compounds)of various kinds,accounting for one third of the total identified structural compounds of the peels.On the contrary,there was only one flavonoid identified in the seeds.A total of 4 components were found both in the nonvolatile component of the ethanol extract in the seeds and peels,including monosaccharides of D-gluconic acid and D-glucopyranuronic acid,disaccharide of sucrose,flavonoid of chysin.The results showed that the nonvolatile components of the seeds were lesser than that of the peels.The chemical co

关 键 词：UPLC-Q-TOF-MS 益智种子和果皮 成分分析 

分 类 号：S567.239[农业科学—中草药栽培]