HPLC-ESI-MS分析紫色小白菜中花色苷组成分析

采用HPLC-ESI-MS方法测定并分析"新紫冠"紫色小白菜中花色苷的组分及其含量。结果表明,"新紫冠"紫色小白菜中含有矢车菊及飞燕草两类花色苷,以矢车菊-3,5-双葡萄糖苷标准品测得总花色苷含量为51.36μg/g·fw,其中矢车菊类花色苷含50.71μg/g·fw,占总含量的98.73%,飞燕草类花色苷含0.65μg/g·fw,仅占1.27%。矢车菊类花色苷全部以酰基化的形式存在,共检测出10种矢车菊类花色苷及相应的9种同分异构体,其中矢车菊-3-阿魏酰-槐糖苷-5-丙二酰-葡萄糖苷是含量最多的花色苷成分,达16.36μg/g·fw,占总含量的31.85%。     

紫玉米苞叶花色苷的纯化鉴定及热稳定性分析

为明确紫玉米苞叶花色苷的组成及比较单体花色苷的热稳定性,实验采用大孔树脂、凝胶树脂分离纯化紫玉米苞叶花色苷提取物,得到三个不同花色苷组分,并采用液质联机的方法鉴定其结构;将制备的花色苷提取物及三个单体组分进行热重仪器分析,比较不同组分的热稳定性结果表明紫玉米苞叶中共含有6种花色苷,通过分离纯化后能够得到三个组分,第一个组分为芍药-3-O-葡萄糖苷和天竺葵-3-O-葡萄糖苷的混合物,第二个组分为矢车菊-3-O-葡萄糖苷,第三个组分为矢车菊-3-(6' 丙二酰-葡萄糖苷).其中总花色苷提取物的热稳定性最强,矢车菊-3-(6'丙二酰-葡萄糖苷)次之,芍药-3-O-葡萄糖苷和天竺葵-3-O-葡萄糖苷的混合物与矢车菊-3-O-葡萄糖苷热稳定性相当,均较以上组分弱.     

紫玉米苞叶花色苷与牛血清白蛋白相互作用研究

采用荧光光谱法、紫外可见吸收光谱法、高效液相色谱法研究紫玉米苞叶花色苷与牛血清白蛋白(BSA)之间的相互作用。结果表明,紫玉米苞叶花色苷与BSA之间存在一定的相互作用,结合程度随着紫玉米苞叶花色苷浓度的增加而增加,二者结合后,会引起BSA结构的变化。紫玉米苞叶中6种主要的花色苷成分与BSA结合程度不同,其结合能力大小依次为:天竺葵-3-(6'-丙二酰葡萄糖苷)芍药-3-(6'-丙二酰葡萄糖苷)天竺葵-3-葡萄糖苷矢车菊-3-葡萄糖苷矢车菊-3-(6'-丙二酰葡萄糖苷)芍药-3-葡萄糖苷。     

加热方法对紫甘蓝花色苷组分及其清除自由基活性的影响

目的:研究蒸汽加热和微波加热处理对紫甘蓝花色苷及其清除自由基活性的影响。方法:采用HPLC-MS法分析花色苷组分,ORAC法评价其清除自由基活性。结果:紫甘蓝花色苷主要有7种组分:矢车菊素-3-槐糖苷-5-葡萄糖苷(组分Ⅰ)、矢车菊素-3-槐糖苷(组分Ⅱ)、芥子酰矢车菊素-3-槐糖苷-5-葡萄糖苷(组分Ⅲ)、芥子酰矢车菊素-3-槐糖苷(组分Ⅳ)、p-香豆酰阿魏酰芥子酰芍药素-3-槐糖苷-5-葡萄糖苷(组分Ⅴ)、芥子酰矢车菊素-3-槐糖苷-5-葡萄糖苷(组分Ⅵ)、二芥子酰矢车菊素-3-槐糖苷-5-葡萄糖苷(组分Ⅶ),其中,组分Ⅰ、Ⅲ、Ⅵ、Ⅶ含量较高。蒸汽加热和微波加热对紫甘蓝花色苷组分种类均无明显影响,而对其相对含量有所影响,微波加热较蒸汽加热对两种花色苷组分Ⅵ和Ⅶ影响显著。蒸汽加热,花色苷组分Ⅵ和Ⅶ分别增加4.46%和10.25%;微波加热,花色苷组分Ⅵ和Ⅶ分别增加10.90%和28.60%。加热后花色苷组分Ⅰ和Ⅲ相对含量有所减少,蒸汽加热两者分别减少2.15%和13.32%,微波加热分别减少6.07%和35.10%。两种加热处理对花色苷组分Ⅱ和Ⅳ相对含量无明显影响。ORAC评价结果表明,微波加热和蒸汽加热对花色苷清除自由基活性有一定的影响,对照组、微波组和蒸汽组的ORAC值分别为0.329±0.030,0.326±0.027,0.293±0.021μmol Trolox/m L。结论:蒸汽加热和微波加热影响紫甘蓝花色苷各组分的相对含量及其清除自由基活性。     

采用HPLC-DAD-ESIMS技术鉴定紫山药中的花色苷成分

采用大孔树酯对浙江台州黄岩紫山药中的花色苷进行分离,并用高压液相色谱-二极管阵列检测-质谱检测技术对其中的主要花色苷进行结构鉴定。通过差异pH法分析紫山药中花色苷的含量为28.8mg/kg。紫山药中4种主要的花色苷可能是:矢车菊素-3-葡萄糖苷或半乳糖苷的双咖啡酸酰化物,矢车菊素-3-二糖苷的芥子酸酰化物,矢车菊素-3-二糖苷阿魏酸的酰化物,芍药色素-3-二糖苷的芥子酸酰化物。     

红树莓花色苷含量测定及成分分析

运用HPLC-DAD-ESI-MS技术建立了测定红树莓花色苷含量的方法,并确定了花色苷的成分组成。采用Zorbax SB-C18色谱柱(250 mm×4.6 mm,5μm),甲醇-5%甲酸水溶液为流动相,流速为1.0 mL/min,检测波长为520 nm,以矢车菊素-3-葡萄糖苷为对照,用外标法定量,并通过紫外扫描光谱信息和ESI+碎片离子信息对花色苷组成成分定性分析。结果表明:红树莓总花色苷含量为105.69 mg/100 g,其主要含有的4种花色苷成分为矢车菊素-3-槐糖苷、矢车菊素-3-槐糖-5-鼠李糖苷、矢车菊素-3-葡萄糖苷、矢车菊素-3-芸香糖苷,相对含量分别为22.05%、13.83%、33.74%和30.38%。     

采用高效液相色谱串联质谱法分析黑粒小麦麸皮中的花色苷组成

以黒粒小麦麸皮为原料,应用高效液相色谱配以串联质谱和二极管阵列检测技术对黒粒小麦中麸皮中的花色苷的组成进行了分析。结果显示:从黒粒小麦麸皮中分离鉴定出9种不同的花色苷类化合物———矢车菊素-己糖苷、矢车菊素-芦丁苷、芍药素-己糖苷、矢车菊素-丙二酰葡萄糖苷、飞燕草素-己糖苷、飞燕草色素-芦丁苷、锦葵色素-芦丁苷、芍药素-芦丁苷及牵牛花素-芦丁苷,其中飞燕草类花色苷和矢车菊素类花色苷是主要花色苷,分别占全部花色苷含量的50.27%和30.04%。     

七种花色苷色素中矢车菊-3-葡萄糖苷含量研究

目的:调查研究七种花色苷色素中矢车菊-3-葡萄糖苷的含量.方法:实验采用高效液相色谱法,检测条件为Ultimate(R)LP-C18(5μm,250mm ×4.6mm)色谱柱;甲酸水溶液(1∶9)∶甲醇=85∶15(v/v)梯度洗脱;流速1mL/min;柱温30℃;检测波长535nm.结果:萝卜红、甘薯红、甜菜红中不含矢车菊-3-葡萄糖苷,葡萄皮色素、欧洲越橘色素、红米红、甘蓝红中矢车菊-3-葡萄糖苷含量分别为5.09％、4.15％、10.84％、0.03％.结论:七种花色苷色素中矢车菊-3-葡萄糖苷含量存在明显差异,葡萄皮色素、欧洲越橘红色素、红米红中矢车菊-3-葡萄糖苷含量较高,为矢车菊-3-葡萄糖苷的进一步开发利用提供了可靠的理论依据.     

欧李花色苷的分离及其鉴定

采用高效液相色谱与离子阱串联飞行时间检测器-质谱联用技术,分离鉴定欧李中的花色苷类化合物。结果表明：从欧李红色素中分离得到6种组分,分别为：矢车菊-3-葡萄糖苷、天竺葵-3-葡萄糖苷、矢车菊-3-鼠李糖葡萄糖苷、天竺葵-3-鼠李糖葡萄糖苷、矢车菊-3-乙酰基葡萄糖苷、天竺葵-3-乙酰基葡萄糖苷。其中,矢车菊-3-葡萄糖苷为主要花色苷,占欧李总花色苷含量的62.6%。因此,采用高效液相色谱-质谱联用技术可有效地分离分析欧李中花色苷类物质。     

超高效液相色谱法测定有色稻米中花色苷的含量

采用盐酸甲醇溶液超声提取有色稻米花色苷,以超高效液相色谱-紫外检测器对有色稻米中主要花色苷矢车菊素-3-O-葡萄糖苷和芍药素-3-O-葡萄糖苷进行定量检测。结果表明,在0. 5～50. 0μg/mL浓度范围内线性关系良好,R~2 0. 999;矢车菊素-3-O-葡萄糖苷回收率在93. 0%～98. 5%,RSD在0. 33%～3. 50%;芍药素-3-O-葡萄糖苷回收率在96. 0%～111. 7%,RSD在0. 42%～2. 18%。对四川重庆地区的4个黑米样品、1个紫米样品和5个红米样品的糙米和米糠中主要花色苷的测定结果表明,黑米、黑米糠、紫米和紫米糠中花色苷总量分别为0～1 051. 27 mg/kg,74. 06～206. 82 mg/kg,296. 18 mg/kg和116. 15 mg/kg;红米中未检出矢车菊素-3-O-葡萄糖苷和芍药素-3-O-葡萄糖苷,部分红米糠中检出矢车菊素-3-O-葡萄糖苷,含量为0～50. 94 mg/kg。     

The effects of six phenolic acids and tannic acid on colour stability and the anthocyanin content of mulberry juice during refrigerated storage

Six phenolic acids and tannic acid are added to fresh mulberry juice to enhance the colour. Effects of these copigments on colour stability and the anthocyanin content of mulberry juice are investigated while being stored at 4 °C for 30 days. Results suggest that the addition of the copigments markedly increases the maximum absorbance of mulberry juice. Cyanidin-3-glucoside is the major anthocyanin, followed by cyanidin-3-rutinoside. Furthermore, the retention rate of the total anthocyanin, cyanidin-3-rutinoside and cyanidin-3-rutinoside increases after the addition of all copigments. The effect of ferulic acid on the stability of total anthocyanin, cyanidin-3-glucoside and cyanidin-3-rutinoside in mulberry juice is the best, 89.52%, 86.90% and 94.46% respectively (66.56%, 62.58% and 73.60% in the control group). Researchers recommend the addition of ferulic acid, p-coumaric acid and caffeic acid – all of which belong to the hydroxycinnamic acid group, to the mulberry juice to enhance the colour stability and anthocyanin content.     

不同品种桑椹酒抗氧化能力及其多酚含量分析

对6个不同品种的桑椹酒的总酚、总类黄酮、原花青素、总花色苷及桑椹酒中主要的两种花色苷（矢车菊-3-氧-芸香糖苷和矢车菊-3-氧-葡萄糖苷）的总抗氧化能力及其相关性进行了分析.结果表明,不同品种的总酚、总类黄酮、原花青素、总花色苷、矢车菊-3-氧-葡萄糖苷、矢车菊-3-氧-芸香糖苷和总抗氧化能力变幅和变异系数较大,存在显著差异（P＜0.05）;桑椹酒总抗氧化能力与总酚、总类黄酮、原花青素、总花色苷及矢车菊-3-氧-葡萄糖苷和矢车菊-3-氧-芸香糖苷含量之间存在正相关性,其中与总酚的相关性最强,达到0.917 2.     

Anthocyanin composition of cauliflower (Brassica oleracea L. var. botrytis) and cabbage (B. oleracea L. var. capitata) and its stability in relation to thermal treatments

Violet cauliflower and red cabbage were analysed for their anthocyanin profiles before and after thermal treatments. Anthocyanins are well-noted as healthy compounds due to their antioxidant properties. Samples were analysed for total anthocyanin content by using a spectrophotometric differential pH method. An MS-based method, combining high-performance liquid chromatography (HPLC) with quadrupole tandem mass spectrometry (HPLC–MS/MS) was developed, aimed to separate, identify and quantify the main anthocyanin forms. The procedure involves a rapid and efficient pre-treatment of the samples by solid-phase extraction, followed by selective determination of all compounds in a single run analysis using HPLC–MS/MS. Structural information for the identification of compounds was obtained from their fragmentation patterns (MS/MS spectra). The compounds were separated by HPLC and detected in the multiple reaction monitoring mode (MRM), which provides a high level of selectivity for targeting the analytes in vegetables. Cauliflower and red cabbage showed differences in their anthocyanin profiles: cyanidin-3,5-diglucoside was absent in cauliflower, while it was well represented in red cabbage, together with the characteristic anthocyanin of Brassica genus, cyanidin-3-sophoroside-5-glucoside. The p-coumaryl and feruloyl esterified forms of cyanidin-3-sophoroside-5-glucoside were predominant in cauliflower, while the sinapyl one was mostly present in red cabbage. Besides, the stability of cauliflower’s anthocyanin profile was evaluated in relation to thermal pre-treatments. All thermal treatments, except microwave heating, drastically reduced total cauliflower anthocyanin content. The amount of individual anthocyanins was expressed as the percentage with respect to total anthocyanin amount, spectrophotometrically measured. Significant individual changes were observed after different thermal treatment with an isomer formation.     

ANTHOCYANIN PIGMENTS OF SOUR CHERRIES

Fresh fruits of tart cherries (Prunus cerasus L. var. Montmorency) were extracted with acidic methanol. The anthocyanin pigments were isolated and purified by conventional paper chromatography. They were identified by spectral and R_f data and by acid hydrolysis. The pigments were cy anidin-3-glucosylrutinoside, cyanidin-3-glucosylsambubioside, cyani-din-3-sophoroside, cyanidin-3-rutinoside, cyanidin-3-glucoside and peoni-din-3-rutinoside. No free cyanidin or peonidin was found. Cyanidin-3-glucosylsambubioside, reported in cherries for the first time, was also found in the varieties of English Morello, Early Richmond and Meteor     

HPLC法测定桃不同品种果实中花色苷组成和含量

目的： 用高效液相色谱法测定桃不同品种果实中花色苷组成和含量。方法： 色谱柱为C1 8柱(150mm×4.6mm,5μm),流动相为乙腈：4%磷酸溶液(V/V=12:88,pH2),检测波长520nm,流速0.8mL/min,进样量20μL,柱温30℃。结果：桃3个品种果实中主要含有1种花色苷：花青素-3-葡萄糖苷,花青素-3-葡萄糖苷在0.4～100μg/mL内线性关系良好(R=0.9992),低、中、高质量浓度的平均回收率为85.7%、89.4%、91.2%。红、黄、白肉桃果肉中的花青素-3-葡萄糖含量分别为103.7、30.6、21.5mg/kg。结论：本方法操作简单,结果准确可靠,重复性好,可作为桃果实中花青素-3-葡萄糖苷的定量分析方法。     

Anthocyanin Pigment Composition of Blackberries

ABSTRACT: The anthocyanin pigments in 51 blackberry samples were isolated and characterized by highperformance liquid chromatography (HPLC) with UV-visible detection, electrospray mass spectroscopy (ESMS), and hydrolysis and saponification reactions. Five pigments were detected: cyanidin-3-glucoside, cyanidin-3-rutinoside, cyanidin-3-xyloside, cyanidin-3-glucoside acylated with malonic acid, and an unidentified acylated derivative of cyanidin-3-glucoside. Four different quantitative patterns were evident among the cultivars and selections. Total anthocyanin content ranged from 70.3 to 201 mg/100 g with a mean of 137 mg/100 g. Ten commercial blackberry juice concentrate samples were analyzed. Total anthocyanin ranged from 12.3 to 107 mg/100 g on a single-strength juice basis, and 1 sample had an atypical profile.     

芽球菊苣根粗多糖提取工艺优化及其体外抗氧化活性和相对分子量分析

目的:以印度芽球菊苣根为原料优化粗多糖的提取工艺,测定其抗氧化性及相对分子量。方法:考察料液比、水浴温度和水浴时间对菊苣根粗多糖得率的影响;采用Box-Behnken结合Matlab分析法优化粗多糖热水浸提法提取工艺;测定所提菊苣根粗多糖体外羟自由基清除能力和还原力;纯化后分析中性糖和酸性糖的平均相对分子量。结果:经过单因素和Box-Behnken设计优化试验,得到最佳提取工艺为:料液比2.74:100 g/mL,水浴温度72 ℃和水浴时间165 min,此时菊苣根粗多糖得率的理论预测值为40.32%,经验证实际值为39.99%±0.43%,与预测值差异不显著（P>0.05）;经Matlab分析,当提取时间取较高值（C=165 min）,料液比2.4:100～3.1:100 mL/g,水浴温度70～74 ℃,粗多糖得率可以取得较大值。按照上述最优工艺所提菊苣根粗多糖具备羟自由基清除能力（IC₅₀值为1.36 mg/mL）和Fe3+还原力（3 mg/mL对应吸光值0.21）,且与浓度呈现正相关。此外,采用高效液相色谱（High Performance Liquid Chromatography,HPLC）测得菊苣中性糖和酸性糖峰型良好,酸性糖峰高且窄表现出较高的纯度,中性糖和酸性糖平均相对分子量分别为10072.07和2388.13 Da。结论:Box-Behnken优化法结合Matlab分析法优化菊苣根粗多糖提取工艺切实可行,所提粗多糖不仅高得率,也兼具良好的体外抗氧化能力,其中,酸性糖纯度较高,中性糖分子量较大。     

Antioxidant assessment of an anthocyanin-enriched blackberry extract

Gel filtration of black berry (Rubus fruticosus sp) ethanolic extracts was employed to obtain an anthocyanin-enriched extract. The anthocyanin profile identified cyanidin-3-glucoside as the primary (e.g., 90% of total) anthocyanin present in blackberry. Gel filtration of crude extracts resulted in a 20-fold increase in total anthocyanin content, with no change in the proportion of cyanidin-3-glucoside. Antioxidant activities of both the crude and anthocyanin-enriched blackberry extracts were determined using cell-free (ORAC) and cell-based (INT-407 intracellular) antioxidant assays. Antioxidant activity, assessed by the ORAC assay, indicated a 7-fold increase in activity for the anthocyanin-enriched fraction. Similar results were obtained for the anthocyanin-enriched extract using the intracellular antioxidant assay with INT-407 cells. Our results indicate that the anthocyanin content, and more specifically the presence of cyanidin-3-glucoside, in blackberry, contributes a major part of the antioxidant ability to suppress both peroxyl radical-induced chemical and intracellular oxidation.     

Anthocyanins in Fruits of Vaccinium oxycoccus L. (Small Cranberry)

Peonidin-3-glucoside (41.9%) and cyanidin-3-glucoside (38.3%) were the main anthocyanins isolated from fruits of Vaccinium oxycoccus L. (Small cranberry). Smaller amounts of the 3-monogalactosides and 3-monoarabinosides of peonidin and cyanidin were found in addition to the 3-monoglucosides of delphinidin, petunidin and malvidin. The total anthocyanin content in the fruit averaged 78 mg/100g fresh fruit. This anthocyanin pattern is different from that of the American cranberry (Vaccinium macrocarpon L.).     

蓝靛果酒发酵工艺优化及发酵过程对花色苷的影响

以蓝靛果为原料,进行蓝靛果酒发酵工艺的优化,并分析发酵过程对花色苷含量及花色苷组成的影响。通过比较不同酵母及不同糖类对果酒总酸、残糖、花色苷含量、乙醇体积分数及感官评分的影响,选择安琪葡萄酒果酒专用酵母SY作为发酵菌,蔗糖作为菌株的碳源,研究酵母接种量、起始pH值和发酵温度对蓝靛果酒理化性质及感官的影响,并在单因素试验的基础上进行3因素3水平的正交试验优化。结果表明,蓝靛果酒发酵的最佳工艺为：接种量0.15%、起始pH?3.2、发酵温度26?℃。在此条件下发酵12?d,乙醇体积分数为9.33%,感官评分为75.15,花色苷质量浓度为80.49?mg/L,为初始花色苷质量浓度（211.0?mg/L）的38.13%。利用高效液相色谱-串联质谱联用测定发酵对花色苷组成及各组成所占比例的影响,结果显示发酵前后的样品中均含有所测的8?种花色苷,发酵后矢车菊素-3-二己糖苷、芍药素-3,5-二己糖苷、矢车菊素-3,5-二己糖苷、芍药素-3-芸香苷、矢车菊素-3-乙酰基乙糖苷及芍药素-3-葡萄糖苷所占峰面积均有所增加,而矢车菊素-3-葡萄糖苷和天竺葵素-3-葡萄糖苷所占峰面积降低。