茶树花多酚大孔树脂纯化工艺研究

该文以废弃茶树花为原料，采用超滤法处理茶树花多酚超声波辅助乙醇浸提液，去除大分子物质，运用静态吸附和动态吸附试验对HZ系列5种大孔吸附树脂及其纯化茶树花多酚工艺条件进行筛选，采用HPLC监测树脂纯化前后茶树花多酚的变化情况。结果表明，HZ-806大孔吸附树脂对茶树花多酚的吸附性能与解吸效果最好，吸附率和解吸率分别达到97.5％、98.20％，适宜作为茶树花多酚纯化的树脂；HZ-806大孔树脂纯化茶树花多酚的工艺条件为：上柱液pH 3.0，上柱液浓度4.0 mg/mL，上柱液体积6 BV，上柱流速4 BV/h，洗脱液乙醇浓度70％，洗脱流速2 BV/h，洗脱体积3.33 BV；采用上述纯化工艺茶树花多酚纯度从19.43％提高到84.32％。     

大孔树脂分离纯化柚皮黄酮的研究

该文以总黄酮含量和总黄酮回收率为考察指标，研究了大孔树脂分离纯化柚皮黄酮的工艺。结果表明：AB-8型树脂对柚皮总黄酮有较好的吸附分离性能，是分离纯化柚皮黄酮的适宜大孔树脂；AB-8型大孔树脂分离纯化柚皮黄酮的最佳工艺条件为：柱体积为160 mL，柚皮提取物上样量为62.5 mg/mL(以湿树脂体积计)，先用pH 4的水淋洗，再用30%的乙醇洗脱，洗脱剂用量为2.5～3倍湿树脂体积。AB-8大孔树脂按上述确定的吸附洗脱条件可重复使用3次。柚皮黄酮经上述工艺纯化后总黄酮含量达到39.67%，总黄酮回收率为62.48%。对经AB-8大孔树脂纯化后的柚皮黄酮进行高效液相色谱(HPLC)分析发现，柚皮黄酮主要为黄酮甙类。     

大孔树脂纯化黄精多酚及其抗氧化性与组成分析

考察4种树脂对黄精多酚粗提物的吸附-解吸特性,筛选出最佳的纯化树脂,并研究其纯化工艺,分析黄精多酚的体外抗氧化活性、红外光谱特性和单酚组成。结果表明,AB-8型大孔树脂最适合于对黄精多酚粗提液的纯化,静态吸附5 h达到饱和,静态解吸3 h达到平衡;在室温下,用质量浓度为0.80 mg/mL的黄精多酚粗提液以0.8 mL/min的流速上样;吸附平衡后以70%的乙醇为洗脱剂,在洗脱流速为1 mL/min时,大孔树脂纯化效果最好,经纯化后黄精多酚的纯度提高了3.37倍。黄精多酚具有较好的抗氧化能力,且具有良好的量效关系,纯化前后黄精多酚总还原能力的IC50值分别为(27.48±1.93)、(19.01±1.48)μg/mL,清除DPPH·的IC50值依次为(5.21±0.48)、(4.00±0.26)μg/mL,清除ABTS+·的IC50值依次为(4.89±0.82)、(4.21±0.53)μg/mL,经纯化后黄精多酚的抗氧化活性明显增强。红外光谱分析表明其具有多酚和黄酮的特征峰;HPLC-DAD分析表明,黄精多酚主要含绿源酸,阿魏酸,芦丁和熊果酸。     

D315树脂分离茶多糖工艺的研究

对D315树脂分离纯化茶多糖的工艺进行了研究,试验结果表明,D315树脂适合用于茶多糖的初步分离和纯化。在上样液pH值6.0～7.0,温度30℃,糖醛酸质量浓度2.5 mg/mL时,先收集上柱吸附的流出液和去离子水洗脱液,得到以中性糖为主的茶多糖NTPS,该多糖总糖质量分数为82.7%,糖醛酸质量分数为7.9%;而后采用0.5 mol/L NaCl溶液洗脱,得到糖醛酸含量高的酸性糖ATPS,该多糖总糖质量分数为85.5%,糖醛酸质量分数为35.2%。     

大孔吸附树脂分离纯化罗汉果皂甙的新方法

该文对大孔树脂分离纯化高含量罗汉果皂甙提取物的新方法进行了研究。结果表明：大孔树脂D101对罗汉果皂甙的分离效果较好,最佳柱分离条件为：上样液pH值9.0,在40℃下依次用pH值9.0的碱水溶液、蒸馏水、30%乙醇及60%乙醇进行洗脱,将60%乙醇洗脱液浓缩,冷冻干燥即得高含量罗汉果皂甙提取物。高效液相分析表明,罗汉果皂甙中几种主要成分的含量均高于分离前的罗汉果皂甙水提物,其中罗汉果皂甙V的含量为69.24%,提高了41.12%。     

大孔吸附树脂分离纯化红小豆多酚工艺及效果

为开发利用红小豆加工副产物中的生理活性物质,该研究采用大孔树脂吸附法对煮制红小豆水的多酚类物质进行分离纯化,比较了5种不同型号大孔树脂对红小豆多酚的吸附分离效果,从中筛选出HPD 600型树脂作为理想的吸附剂;研究了 HPD 600树脂对红小豆多酚的吸附等温线,结果表明,该吸附等温线与 Langmuir、Freundlich函数曲线的拟合程度非常高,且采用Langmuir模型的拟合效果略优于Freundlich模型。静态和动态吸附、洗脱试验结果表明：样品液浓度、温度、pH值、乙醇浓度、上样流速及洗脱流速等因素均对HPD 600树脂吸附分离红小豆多酚有影响。较理想的工艺参数为：30℃是较适宜的静态吸附温度;保持煮制红小豆水本身的多酚浓度0.96 mg/mL和pH值6.8,上样体积200 mL,上样流速1.0 mL/min进行动态吸附;吸附饱和平衡后,采用50 mL 60%乙醇溶液,以1.5 mL/min的流速进行动态洗脱。依此得到的红小豆多酚纯化液,其总酚含量和总抗氧化能力均有显著提高,约为纯化前的2.2倍。     

油梨皮黄酮提取及大孔树脂纯化

该文研究了油梨皮黄酮的提取及大孔树脂纯化条件.结果表明:油梨皮黄酮的最佳提取条件为乙醇浓度70%、提取温度70℃、提取时间1.5 h、料液比(m/V)1:20.乙醇浓度和提取温度对提取得率有显著性(P<0.05)影响.在此条件下,黄酮的提取得率为1.12%;AB-8型树脂对油梨皮黄酮有较好的吸附和洗脱效果,其纯化油梨皮黄酮的条件为柱体积250 mL,上样量2.03 g,水洗,接着用75%的乙醇洗脱(约500 mL),在此条件下AB-8型树脂可重复使用6次.经纯化后油梨皮黄酮相对纯度为82.37%,纯化后总黄酮回收率为71.65%.     

大孔树脂分离纯化玫瑰果多酚及其抗氧化性

为了研究大孔树脂对玫瑰果多酚的纯化效果,该试验以玫瑰果多酚粗提液为原料,利用大孔树脂吸附法对其进行纯化,并对其体外抗氧化活性进行了研究。结果表明,大孔吸附树脂纯化较佳工艺为:在20℃条件下,用质量浓度为0.80 mg/m L的玫瑰果多酚粗提液(p H值5.8)以1 m L/min的流速上样200 m L;吸附平衡后用少量蒸馏水洗至洗脱液无色,后用70 m L体积分数为70%的乙醇溶液,以1.5 m L/min的流速进行动态洗脱,洗脱峰相对集中、对称,无拖尾。纯化后,总酚质量分数由纯化前的122.90 mg/g提高到399.42 mg/g。体外抗氧化活性的研究表明:清除1,1-二苯基-2-苦基肼自由基的作用效果顺序为维生素C纯化多酚2,6-二叔丁基-4-甲基苯酚(Butylated hydroxytoluene,BHT)粗多酚;清除超氧阴离子自由基的作用效果顺序为维生素CBHT纯化多酚粗多酚;清除羟基自由基的作用效果顺序为维生素C纯化多酚BHT粗多酚。研究结果为玫瑰果多酚的进一步利用提供依据。     

血橙花色苷大孔树脂纯化工艺及抗氧化研究

研究了D101、HPD-300、NKA-9和AB-8四种大孔树脂富集纯化血橙花色苷的性能和分离特性,发现D101是纯化血橙花色苷较适合的树脂类型。为了优化工艺,在D101大孔树脂上进行了静态和动态的吸附和解吸实验,结果表明:血橙汁在D101大孔树脂的上样体积为10 BV,吸附平衡时间2 h;选择pH值为2的60%乙醇进行洗脱,洗脱体积为8 BV。经纯化后得到的血橙花色苷为深红色粉末,色价为48.4。血橙花色苷具有较好的抗氧化性能,在一定的浓度范围内,对DPPH和ABTS自由基有一定的清除作用,其作用随浓度的增加而增强。     

鱼腥草叶总黄酮的提取分离

采用微波辅助提取鱼腥草叶总黄酮,并用正交试验进行工艺参数的优化。同时选择7种大孔树脂,比较其对鱼腥草叶总黄酮的吸附量和解吸率,筛选出较优的大孔树脂并对其动态吸附及解吸性能进行考察。结果表明:优化的工艺条件为乙醇浓度50%,固液比1∶50(w/v),预浸泡30 min,微波作用时间30 s,微波功率540 W;与传统乙醇提取法相比,微波法使每次提取时间由3 h减少为30.5 min,提取率从92.14%增加到95.93%。NKA-9型大孔树脂对鱼腥草叶总黄酮有较好的吸附和解吸效果;较优的吸附分离工艺参数为:样液pH值在3.00～3.50,上样液流速1 mL/min,上样液浓度2.21～3.10 mg/mL,用70%乙醇洗脱时,解吸率达97.8%,3BV洗脱液基本上能将鱼腥草叶总黄酮洗脱下来。     

大孔树脂对苹果渣中多酚物质的吸附研究

通过静态吸附与解吸实验对8种大孔树脂进行筛选,结果表明:NKA-9型大孔树脂表现出最好的吸附性能与解吸效果,是较好的富集纯化苹果多酚树脂。通过单因素实验，确定NKA-9树脂的较佳动态吸附条件为苹果多酚液浓度2.50 mg/mL，pH 4.5，流速1.0 mL/min，较佳洗脱条件为乙醇浓度60%,洗脱流速1.0 mL/min,洗脱体积10 BV。     

Development of a solid-phase extraction method for phenoxy acids and bentazone in water and comparison to a liquid-liquid extraction method

A rapid solid-phase extraction (SPE) method was developed for the determination of bentazone and the phenoxy acids 2,4-D, dichlorprop, MCPA, and mecoprop in Norwegian environmental water samples. Cartridges with a high-capacity cross-linked polystyrene-based polymer were used for off-line preconcentration. The effects of elution solvent, elution volume, sample volume, sorbent mass, pH, and flow rate on the recoveries of the pesticides were investigated using HPLC. Average recovery of >90% was achieved with 500 mg sorbents using 2 mL of methanol with 5% NH3 as elution solvent. The recoveries were independent of sample pH in the tested range of pH 1-7. Using a sample volume of 200 mL, the limits of determination for the phenoxy acids and bentazone are 0.02 microg/L. Sample volumes up to 2000 mL at a flow rate of 60 mL/min could be handled without any loss of analytes, which makes it possible to lower the limits of determination. The SPE method was compared to a routinely used liquid-liquid extraction method. Three different water matrices spiked at 1.0 and 0.05 microg/L were extracted, and the quantification was performed by GC-MS. Both methods permitted the determination of phenoxy acids and bentazone in distilled water, creek water, and well water down to a level of 0.05 microg/L with recoveries >80% for 200 mL samples. Important advantages of the SPE method compared to the liquid-liquid extraction method were the short extraction times, lack of emulsions, use of disposable equipment, and reduced consumption of organic solvents.     

Evaluation of antioxidant activity and preventing DNA damage effect of pomegranate extracts by chemiluminescence method

The antioxidant activities of three parts (peel, juice, and seed) and extracts of three pomegranate varieties in China were investigated by using a chemiluminescence (CL) method in vitro. The scavenging ability of pomegranate extracts (PEs) on superoxide anion, hydroxide radical, and hydrogen peroxide was determined by the pyrogallol-luminol system, the CuSO4-Phen-Vc-H2O2 system, and the luminol-H2O2 system, respectively. DNA damage preventing the effect of PE was determined by the CuSO4-Phen-Vc-H2O2-DNA CL system. The results showed that the peel extract of red pomegranate had the best effect on the scavenging ability of superoxide anion because its IC50 value (4.01 +/- 0.09 microg/mL) was the lowest in all PEs. The seed extract of white pomegranate could scavenge hydroxide radical most effectively of the nine extracts (the IC50 value was 1.69 +/- 0.03 microg/mL). The peel extract of white pomegranate had the best scavenging ability on hydrogen peroxide, which had the lowest IC50 value (0.032 +/- 0.003 microg/mL) in the nine extracts. The seed extract of white pomegranate (the IC50 value was 3.67 +/- 0.03 microg/mL) was the most powerful on the DNA damage-preventing effect in all of the PEs. Also, the statistical analysis indicated that there were significant differences (at P < 0.05) among the extracts of the different varieties and parts in each system.     

石榴皮提取液对草莓的保鲜效果

为了发展草莓贮藏保鲜的新技术和有效利用石榴皮资源,以新鲜草莓为材料,在贮藏前分别经过1.25%壳聚糖溶液（T1）、1%石榴皮提取液（T2）、1.25%壳聚糖石榴皮提取物复合溶液（T3）浸泡处理,以蒸馏水浸泡作为对照（CK）,通过对其在贮藏期相关品质指标（质量损失率、软化腐烂率、可溶性固形物质量分数、可滴定酸质量分数、Vc质量分数、丙二醛（MDA）含量）的测定,比较了3种处理溶液的保鲜效果。结果显示,T1、T2、T3处理均降低了草莓果实质量损失率、软化腐烂率和MDA含量,延缓了果实可滴定酸、可溶性固形物和Vc质量分数的下降,其中T3处理效果明显好于T1和T2处理,T3处理可使在室温下放置的草莓保鲜期延长1～2 d。结果表明石榴皮提取液用于草莓保鲜可行,与一定浓度的壳聚糖配制的复合保鲜液保鲜效果更理想。     

Determination of lignans in edible and nonedible parts of pomegranate (Punica granatum L.) and products derived therefrom, particularly focusing on the quantitation of isolariciresinol using HPLC-DAD-ESI/MSn

A method for the characterization and quantitation of phyto-estrogenic lignans from pomegranate (Punica granatum L.) fruits and fruit-derived products by HPLC-DAD-MS(n) was developed. For this purpose, edible and nonedible parts of pomegranate (aril, peel, mesocarp, seed, and twigs), commercial juices, juices produced on pilot-plant scale, and encapsulated dietary supplements were analyzed. In addition to the peel, mesocarp, and twigs, lignans were detected in two juices obtained from entire fruits, four commercial juices, and three encapsulated pomegranate extracts. Isolariciresinol was the predominant lignan with contents of 5.0, 10.5, and 45.8 mg/kg dry matter in processed pomegranate mesocarp, peel, and twigs, respectively. In contrast, due to their low amounts, quantitation of lignans in pomegranate products was impossible. Therefore, contrary to previous assumptions, lignans were found to be less relevant in pomegranate-derived products. However, the byproduct from pomegranate processing may be used for lignan extraction. The method presented allows one to differentiate between pomegranate-derived products obtained from fruits without peels or by dejuicing applying low pressures, which were devoid of lignans, and those obtained from entire fruits applying high pressures, thus containing lignans. Consequently, this study helps to optimize process technology aiming at the recovery of preparations with well-desired compositions, which may reduce the risk of a wide range of diseases, such as certain types of cancer.     

不同氮肥用量对石榴果实产量和品质的影响

以‘秋艳’石榴为试验材料,研究了不同氮肥用量对其果实产量和品质的影响。结果表明,施用氮肥可显著提高石榴果实产量,适量施用氮肥可增加石榴果实可溶性固形物、Vc、糖含量,降低石榴果实酸含量,提高石榴果实糖酸比,改善石榴果实的风味;施用氮肥对石榴百粒重、籽粒硬度无显著影响;石榴籽氮元素含量高于石榴皮,石榴汁中氮含量很低,中高氮处理的石榴汁中氮元素含量显著降低,石榴皮和石榴籽中氮元素含量变化不显著;本试验5年生石榴树纯氮施肥用量宜以0.4 kg·株~(-1)为宜。     

Studies on antioxidant activity of pomegranate (Punica granatum) peel extract using in vivo models

Pomegranate (Punica granatum) peel extracts have been shown to possess significant antioxidant activity in various in vitro models. Dried pomegranate peels were powdered and extracted with methanol for 4 h. The dried methanolic extract was fed to albino rats of the Wistar strain, followed by carbon tetrachloride (CCl4), and the levels of various enzymes, such as catalase, peroxidase, and superoxide dismutase (SOD), and lipid peroxidation were studied. Treatment of rats with a single dose of CCl4 at 2.0 g/kg of body weight decreases the levels of catalase, SOD, and peroxidase by 81, 49, and 89% respectively, whereas the lipid peroxidation value increased nearly 3-fold. Pretreatment of the rats with a methanolic extract of pomegranate peel at 50 mg/kg (in terms of catechin equivalents) followed by CCl4 treatment causes preservation of catalase, peroxidase, and SOD to values comparable with control values, wheres lipid peroxidation was brought back by 54% as compared to control. Histopathological studies of the liver were also carried out to determine the hepatoprotection effect exhibited by the pomegranate peel extract against the toxic effects of CCl4. Histopathological studies of the liver of different groups also support the protective effects exhibited by the MeOH extract of pomegranate peel by restoring the normal hepatic architecture.