平榛叶中黄酮类化合物成分的研究

利用高效液相色谱电喷雾离子化串联二级质谱(HPLC-ESI-MS/MS)技术,根据保留时间、母离子和二级质谱碎片与标准品或参考文献比对,对平榛叶黄酮成分进行了定性分析;通过多反应监控模式(MRM)对平榛叶黄酮成分进行了定量分析。共从中鉴定出12种化合物,其中11种为首次从平榛叶中发现,分别为表儿茶素(41.45±1.87μg/g,干叶)、绿原酸(3-咖啡酰奎宁酸,389.00±17.15μg/g)、丁香亭-3-O-葡萄糖苷(6169.78±209.73μg/g)、丹酚酸C(443.37±21.07μg/g)、金圣草黄素-6-C-葡萄糖苷(206.81±10.07μg/g)、金丝桃苷(槲皮素-3-O-半乳糖苷,154.44±7.63μg/g)、槲皮苷(槲皮素-3-O-鼠李糖苷,937.15±40.86μg/g)、西伯利亚落叶松黄酮-3-O-半乳糖苷(17.27±0.82μg/g)、锦葵色素-3-O-葡萄糖苷(202.74±10.04μg/g)、西伯利亚落叶松黄酮-3-O-葡萄糖苷(101.27±4.99μg/g)和山奈酚-3-O-鼠李糖苷(112.37±4.77μg/g)。     

HPLC法同时测定枣叶中5种黄酮的含量

建立了一种枣叶中黄酮类成分定量分析的HPLC方法,并对14个品种的大枣及酸枣叶中这5种黄酮的含量进行了分析。结果得到采用Hypersil BDS C18色谱柱,以乙腈与0.1%甲酸水溶液为流动相梯度洗脱,流速1 m L/min,柱温30℃,检测波长360 nm,实现了槲皮素-3-O-洋槐糖苷、芦丁、槲皮素-3-O-β-D-葡萄糖苷、山奈酚-3-O-芸香糖苷、槲皮素-3-O-α-L-阿拉伯糖-(1→2)-α-L-鼠李糖苷5种黄酮苷的同时检测,最低检出限为1.44~2.59μg/m L,加标回收率在93.8%~105.9%之间。5种黄酮苷的含量测定结果表明不同品种的枣叶中黄酮类成分的组成和含量差异较大,其中芦丁和槲皮素-3-O-洋槐糖苷的含量较高,平均为7.83 mg/g D.W和4.61 mg/g D.W;8个品种枣叶中检测到槲皮素-3-O-α-L-阿拉伯糖-(1→2)-α-L-鼠李糖苷,平均5.32 mg/g D.W;而槲皮素-3-O-β-D-葡萄糖苷和山奈酚-3-O-芸香糖苷的含量较低,分别为0.14 mg/g D.W和0.41 mg/g D.W。     

β-葡萄糖苷酶生物转化刺梨槲皮素糖苷的工艺优化

以不同来源的β-葡萄糖苷酶水解刺梨槲皮素-3-O-芸香糖苷、槲皮素-3-O-鼠李糖苷和槲皮素-3-O-葡萄糖苷,探讨提高刺梨黄酮苷元释放能力的生物转化途径。以槲皮素含量与糖苷转化率为指标,采用高效液相色谱法对来源于嗜酸乳杆菌、木霉和杏仁的β-葡萄糖苷酶水解3种槲皮素糖苷的转化率及槲皮素含量进行动态监测,以酶解时间、酶解pH值、酶解温度和酶用量(酶与底物质量比)为单因素,考察各因素参数独立变化对指标的影响,再以Box-Behnken 方法研究各因素及其交互作用对转化率的影响,优化工艺条件。杏仁β-葡萄糖苷酶水解3种糖苷转化所得槲皮素含量最高,对不同底物的转化率由高到低依次为槲皮素-3-O-葡萄糖苷(74.10%)、槲皮素-3-O-芸香糖苷(64.30%)、槲皮素-3-O-鼠李糖苷(31.80%)。杏仁β-葡萄糖苷酶优化水解工艺条件为酶解时间28.90min,酶解pH值4.9,酶解温度52℃,酶用量0.08%。此条件下得到槲皮素-3-O-芸香糖苷转化率71.48%,槲皮素-3-O-鼠李糖苷转化率36.32%,槲皮素-3-O-葡萄糖苷转化率77.86%。     

甜叶菊花和叶中酚类成分分析及含量测定

以高效液相色谱-串联四极杆质谱分析仪,结合质谱分析及比对对照品或文献报道化合物的保留时间和质谱参数,在甜叶菊花和叶中鉴定了16种酚类化合物。建立一种利用高效液相色谱法测定甜叶菊中16种酚类化合物含量的方法,并对甜叶菊一新品种盛花期花和叶中酚类的含量进行测定。结果表明,甜叶菊花和叶中酚酸化合物以新绿原酸、绿原酸、隐绿原酸、异绿原酸B、异绿原酸A、异绿原酸C为主,异绿原酸A含量最高,绿原酸含量次之;花和叶中类黄酮化合物主要为芦丁、槲皮素-7-O-葡萄糖苷、木犀草素-7-O-葡萄糖苷、木犀草素-7-O-芸香糖苷、槲皮素-3-O-木糖苷、槲皮素-3-O-鼠李糖苷、芹菜素-7-O-葡萄糖苷、山奈酚-3-O-阿拉伯糖苷、山奈酚-3-O-鼠李糖苷,槲皮素-3-O-鼠李糖苷含量最高;盛花期甜叶菊花和叶中酚类总量达（22.31±0.51）mg/g和（91.11±2.32）mg/g。     

高效液相色谱-串联质谱测定砀山酥梨中的酚类物质

本文研究了高效液相色谱-电喷雾串联质谱定性、定量检测砀山酥梨及其制品中的酚类物质。样品中的酚类物质在70min内得到分离,酚类物质由色谱的保留时间、质谱信息和参考文献确定。质谱检测在负离子模式下,利用全扫描模式、多反应检测模式和中性丢失模式进行。本研究在砀山酥梨中共检出酚类27种,主要酚类物质是绿原酸,含量为180mg/L,其次为熊果苷、没食子酸、咖啡酸、咖啡奎宁酸、表儿茶素、儿茶素、柚(皮)苷、芦丁、槲皮素-葡萄糖苷、槲皮素-半乳糖苷、槲皮素-鼠李糖苷、香豆酸-葡萄糖苷、槲皮素-戊糖苷、鼠李糖素-葡萄糖苷、槲皮素等。     

青钱柳叶黄酮的分离纯化与抗氧化性研究

青钱柳黄酮具有丰富的生物活性功能,引起国内外学者的广泛关注。青钱柳叶黄酮提取液经过AB-8型大孔吸附树脂吸附纯化后,然后再由葡聚糖凝胶柱对其黄酮类化合物层析,之后用制备型高效液相色谱(HPLC)制备、纯化,得到3个黄酮类化合物,分别记为化合物Ⅰ、Ⅱ和III。利用高效液相色谱、液质联用技术和核磁共振对上述分离得到的3种黄酮类化合物进行分析鉴定,结果表明:这3种物质分别为槲皮素-3-O-葡萄糖苷,又名异槲皮素(Quercetin-3-O-β-Dglucoside,Isoquercitrin)、槲皮素-3-O-β-D-吡喃半乳糖苷,又名金丝桃甙(Quercetin-3-O-β-Dgalactoside,Hyperin)和山柰酚-3-O-β-D-葡萄糖甙(Kaempferol-3-O-β-D-glucoside)。特别是首次从青钱柳叶中提取到金丝桃甙和山柰酚-3-O-β-D-葡萄糖甙。抗氧化试验结果显示提取的3种青钱柳黄酮有很强的抗氧化能力。     

新疆野生樱桃李(Prunus cerasifera)叶黄酮类成分研究

此项目研究了新疆野生樱桃李叶乙酸乙酯活性部位中的黄酮类化学成分。采用甲醇浸泡提取野生樱桃李叶,依次采用环己烷、乙酸乙酯和正丁醇萃取其醇提物。乙酸乙酯活性部分采用MCI (Middle Chromatogram Isolated Gel)大孔树脂柱粗分离,后续进一步采用硅胶柱、Sephadex LH-20凝胶柱,ODS (Octadecyl silane)反向硅胶柱和制备HPLC等色谱技术对其进行分离纯化,并根据化合物理化性质和核磁共振波谱(NMR)数据并与相关参考文献比对鉴定化合物结构。从野生樱桃李叶中共分离并鉴定11个黄酮类化合物,分别为:槲皮素-3-O-α-L-呋喃阿拉伯糖苷(1),槲皮素-3-O-β-D-木糖苷(2),槲皮素-3-O-β-D-半乳糖苷(3),槲皮素-3-O-α-L-鼠李糖苷(4),山柰酚-3-O-α-L-呋喃阿拉伯糖苷(5),山柰酚-3-O-β-D-木糖苷(6),山柰酚-3-O-β-D-葡萄糖苷(7),山柰酚-3-O-α-L-鼠李糖苷(8),反式-二氢山柰酚-3-O-α-L-鼠李糖苷(9),顺式-二氢山柰酚-3-O-α-L-鼠李糖苷(10),顺式-二氢山柰酚-3-O-β-D-葡萄糖苷(11)。所有黄酮类成分均为首次从新疆野生樱桃李叶中分离鉴定,槲皮素和山柰酚糖苷是其主要的黄酮类成分。     

勿忘我花色素的分离与鉴定

采用超声波强化溶剂法提取了蓝紫色勿忘我花色素,提取溶剂为55%~60%的酸性乙醇溶液。色素平均得率15%,色价(540nm)为36.55。色素经纸色谱(PC)分离主要含有黄色和红色两种物质,特别地对纸色谱分离出的这两种物质进行了显色反应、紫外可见光谱(UV)、红外光谱(IR)的测定分析,认为黄色物质为黄酮类化合物,红色物质为花青素。色素经液相色谱(HPLC)分离,主要含有7个组分,相对含量分别为63.45%、25.45%、0.59%、0.64%、4.27%、5.44%、0.21%。色素经液相色谱-质谱(LC-MS)联用仪的分离测定和结构分析,结果表明蓝紫色勿忘我花色素中含有矢车菊及其葡萄糖苷、黄酮及其衍生物,可能含有少量的飞燕草素和芍药定及其苷。     

枣叶黄酮类成分的分离鉴定及其抗氧化活性研究

对枣叶的乙醇提取物经乙酸乙酯萃取、高效液相色谱反复制备纯化,得到5种化合物。经LC-MS、1H NMR和13C NMR进行鉴定,分别为:槲皮素-3-O-洋槐糖苷(1)、槲皮素-3-O-芸香糖苷(2)、槲皮素-3-O-β-D-葡萄糖苷(3)、山奈酚-3-O-芸香糖苷(4)、槲皮素-3-O-α-L-阿拉伯糖-(1→2)-α-L-鼠李糖苷(5)。对5种黄酮单体化合物清除ABTS+、DPPH自由基的活性进行了比较,结果表明5种化合物清除ABTS+、DPPH自由基的活性呈现出相同的趋势,其中化合物3表现出最强的活性,化合物1、2、5活性适中,化合物4的活性最低。     

液质联用分离测定山西苦荞黄酮

采用液质联用仪对山西苦荞中的黄酮类化合物进行分离鉴定,发现山西灵丘地区产的苦荞提取液中黄酮类化合物以芦丁为主;并分离出5种黄酮类化合物,分别为六取代黄酮(万寿菊素-葡萄糖醛酸苷),槲皮素-3-芸香糖葡萄糖苷,芦丁、槲皮素和槲皮素-3-双鼠李糖苷,其中六取代黄酮(万寿菊素-葡萄糖醛酸苷)和槲皮素-3-双鼠李糖苷为首次发现;并测定出这5种黄酮类化合物的含量分别为3.03%、5.05%、63.23%、4.19%和6.19%.     

会东块菌香气成分的GC-MS分析

采用超声溶剂萃取、同时蒸馏萃取、固相微萃取3种方法对会东块菌香气进行提取后,用气相色谱-质谱联用(GC-MS)法结合计算机检索对其进行成分分析和鉴定。结果表明：采用超声溶剂萃取法的萃取物中共分离出80个峰,鉴定出65种化合物,占总组分的93.59%;用同时蒸馏萃取法的萃取物中共分离出了91个峰,鉴定出了67种化合物,占总组分的90.45%;用固相微萃取法的萃取物中共分离出64个峰,鉴定出50种化合物,占总组分的75.15%;综合比较,采用3种方法共分离鉴定出142种香气物质,其中主要香气物质23种,3种提取方法中同时蒸馏萃取法效果最优。     

花椒精油及其水提物的香气活性成分分析

本研究通过水蒸气蒸馏法提取汉源青花椒、金阳青花椒、汉源红花椒、武都红花椒的挥发性油,采用直接进样法分析花椒精油,采用溶剂辅助蒸发（solvent-assisted flavor evaporation, SAFE）分离花椒水提物中的挥发性成分,结合气相色谱-质谱联用仪（gas chromatography-mass spectrometry, GC-MS）和气相-嗅闻仪（gas chromatography-olfactometry, GC-O）对两者的香气活性成分进行分析。结果显示,在精油和水提物中分别鉴定出99种和153种挥发性成分,仅水提物中含内酯类和酸类物质;青花椒精油及水提物中相对含量最高的物质为芳樟醇、D-柠檬烯、桧烯、萜品烯-4-醇;红花椒精油及水提物中相对含量最高的物质为芳樟醇、D-柠檬烯、乙酸芳樟酯、α-月桂烯;酯类物质含量的差异可能是造成红花椒与青花椒的精油和水提物香气差异的原因。感官评价结果显示,精油的青香、椒麻和油脂味比水提物更强,水提物的甜香、酸味和哈喇味比精油更突出。通过GC-O分析,在精油中和水提物中分别鉴定出57种和68种香气活性物质,经偏最小二乘法（partial least squares regression, PLSR）进行香气属性和化合物的相关性分析,确定了对精油和水提物香气轮廓影响较大的29种物质。     

Structural Identification and Antioxidant Properties of Major Anthocyanin Extracted from Omija (Schizandra chinensis) Fruit

ABSTRACT:  Omija ( Schizandra chinensis ) is used as an ingredient in traditional medicine in East Asia. It is consumed as tea and wine and display pinkish-red color and beneficial physiological activity. However, the origin of Omija's unique color and bioactivity has not been studied extensively and its application is very limited. Thus, it was required to determine the chemical structure of major phenolic compounds of Omija fruit and evaluate their antioxidant activity. The colorants extracted from a domestic Omija cultivar were concentrated by a Sep-pak® Plus C₁₈ cartridge. A major high-performance liquid chromatography (HPLC) peak of anthocyan represented 94.1% of total absorbable compounds at 520 nm, which was further identified by LC-ESI-MS. The mass-to-charge ratio ( m/z ) of the major anthocyan was determined to be 727. Highly pure anthocyan fraction with a semipreparative HPLC was acid-hydrolyzed, and the sugar moieties linked to anthocyan (cyanidin) were characterized by thin layer chromatography (TLC) and high-performance anion exchange chromatography (HPAEC) analyses. The linkage patterns of sugars and core cyanidin structure were determined by ¹H- and ¹³C-NMR analyses. Antioxidant activity of the extract and the purified anthocyanin was evaluated by 1,1-diphenyl-2-picrylhydrazyl (DPPH) and 2,2'-azino-bis(3-ethylbenzthiazoline-6-sulphonic acid) (ABTS) methods. As a result, the structure of the purified colorant was identified as Cya-3- O -xylrut. At the same molar level of the samples tested, the purified Cya-3- O -xylrut (31.2% and 39.2%) had substantially greater antioxidant activity than l -ascorbic acid (17.1% and 10.1%) from DPPH and ABTS methods, respectively. In this study, Omija colorant mostly consisted of Cya-3- O -xylrut explained 86% (DPPH) and 98% (ABTS) of total antioxidant activity derived from water extract from Omija.     

Influence of Fermentation Process on the Anthocyanin Composition of Wine and Vinegar Elaborated from Strawberry

Anthocyanins are the major polyphenolic compounds in strawberry fruit responsible for its color. Due to their sensitivity, they are affected by food processing techniques such as fermentation that alters both their chemical composition and organoleptic properties. This work aims to evaluate the impact of different fermentation processes on individual anthocyanins compounds in strawberry wine and vinegar by UHPLC‐MS/MS Q Exactive analysis. Nineteen, 18, and 14 anthocyanin compounds were identified in the strawberry initial substrate, strawberry wine, and strawberry vinegar, respectively. Four and 8 anthocyanin compounds were tentatively identified with high accuracy for the 1st time to be present in the beverages obtained by alcoholic fermentation and acetic fermentation of strawberry, respectively. Both, the total and the individual anthocyanin concentrations were decreased by both fermentation processes, affecting the alcoholic fermentation to a lesser extent (19%) than the acetic fermentation (91%). Indeed, several changes in color parameters have been assessed. The color of the wine and the vinegar made from strawberry changed during the fermentation process, varying from red to orange color, this fact is directly correlated with the decrease of anthocyanins compounds.     

GC–MS and GC–olfactometry analysis of aroma compounds in a representative organic aroma extract from cured vanilla (Vanilla planifolia G. Jackson) beans

Volatile compounds from cured vanilla beans were extracted using organic solvents. Sensory analysis showed that the aromatic extract obtained with a pentane/ether (1/1 v/v) solvent mixture provided the extract most representative of vanilla bean flavour. Sixty-five volatiles were identified in a pentane/ether extract by GC–MS analysis. Aromatic acids, aliphatic acids and phenolic compounds were the major volatiles. By GC–O analysis of the pentane/ether extract, 26 odour-active compounds were detected. The compounds guaiacol, 4-methylguaiacol, acetovanillone and vanillyl alcohol, found at much lower concentrations in vanilla beans than vanillin, proved to be as intense as vanillin.     

同时蒸馏萃取结合GC-MS分析红托竹荪挥发性成分

采用同时蒸馏萃取法提取红托竹荪中的挥发性成分,用气相色谱一质谱联用（GC—MS）对挥发性成分进行了分析。结果表明通过双柱定性,以乙醚为溶剂时鉴定出81种成分,以二氯甲烷为溶剂时鉴定出89种成分;两种溶剂共计鉴定出108种挥发性成分,其中醛类11种、酮类8种、醇类9种、酚类2种、酯类15种、酸类23种、烃类17种、杂环类17种、其他类6种,其中含量较大的有亚油酸、棕榈酸、棕榈油酸、十五烷酸、11-顺-十八碳烯酸、醋酸、乙偶姻、肉豆蔻酸、十五碳酸、天然麝香葵子等。     

液液萃取结合气-质联机分析景芝白干酒中的挥发性成分

采用不同的溶剂,通过液液萃取法结合气-质联机对景芝白干酒中的香气成分进行分析,并通过NIST 11 谱库 检索和保留指数进行了鉴定。结果表明,不同种类和极性的有机溶剂,其萃取出来的成分也不相同。采用正戊烷作为 萃取剂,共发现30 种物质,采用乙醚作为萃取剂,共发现29 种物质,采用二氯甲烷作为萃取剂,共发现35 种物质。 3 种溶剂一共萃取出65 种物质,其中醇类化合物9 种、酯类化合物19 种、酸类化合物11 种、烃类化合物14 种、芳香 族化合物3 种、呋喃类化合物3 种、醛类化合物3 种、酮类化合物1 种、含氮化合物1 种、含硫化合物1 种。     

芡种壳提取物多酚组成及对猪肉乳化肠贮存期质量的影响

采用50%乙醇溶液从芡实种壳中得到一种提取物(ESE),采用HPLC-UV法对其中的酚类物质组成进行分析,并对其在肉制品保鲜方面的作用进行初步研究。结果表明：ESE中含有丰富的多酚物质,可定性的有没食子酸(364.11mg/g)、绿原酸(42.31mg/g)、表儿茶素(95.95mg/g)、表儿茶素没食子酸酯(3.16mg/g)和芦丁(129.21mg/g)。肉制品保鲜实验表明,单独添加ESE(500mg/kg),可以显著减轻猪肉乳化肠贮存期间的脂类氧化,但不能有效抑制产品pH值升高和改善产品颜色。将ESE、NaNO2和红曲粉进行适当复配,可以有效改善肉制品颜色、抑制其褪色,减轻脂类氧化,并延缓产品pH值升高。结果表明：这3者之间在抑制肉制品中微生物生长和脂类氧化方面存在一定的协同作用。     

岭南山竹子果实的化学成分分离与确定

目的：通过高效液相色谱-飞行时间质谱法对岭南山竹子果实的化学组分进行分析。方法：利用硅胶柱色谱、凝胶柱色谱、高速逆流色谱、高效液相色谱等分离和纯化化合物,并以核磁共振确定化合物的结构。结果：基于高效液相色谱-飞行时间质谱法的分析,初步鉴定了11 个化合物,主要为双黄酮类和多戊异烯基取代的苯甲酮类。提取分离得到5 个化合物,分别鉴定为：oblongifolin C（1）、oblongifolin A（2）、volkensiflavone（3）、GB-1a（4）和β-谷甾醇（5）。结论：从该植物中分离得到化合物3和化合物4,确定岭南山竹子果实的化学成分,可为开发该热带水果提供数据参考。     

Optimization of microwave-assisted extraction of anthocyanins from mulberry and identification of anthocyanins in extract using HPLC-ESI-MS

Anthocyanins are naturally occurring compounds that impart color to fruits, vegetables, and plants. This study aims to optimize the microwave-assisted extraction (MAE) conditions of anthocyanins from mulberry (M. atropurpurea Roxb.) using response surface methodology (RSM). A Box-Behnken experiment was employed in this regard. Methanol concentration, microwave power, and extraction time were chosen as independent variables. The optimized conditions of MAE were as follows: 59.6% acidified methanol, 425 W power, 25 (v/w) liquid-to-solid ratio, and 132 s time. Under these conditions, 54.72 mg anthocyanins were obtained from 1.0 g mulberry powder. Furthermore, 8 anthocyanins were identified by high-performance liquid chromatography-electrospray ionization-mass spectrometry (HPLC-ESI-MS) in mulberry extract. The results showed that cyanidin-3-glucoside and cyanidin-3-rutinoside are the major anthocyanins in mulberry. In addition, in comparison with conventional extraction, MAE is more rapid and efficient for extracting anthocyanins from mulberry.