柱色谱分离制备低乙酸乙酯儿茶素

儿茶素作为绿茶的标志性活性物质,它的提取和制备技术一直以来备受关注。本文在前人研究的基础上,以绿茶碎末为原料,经溶剂浸提、离心除渣、柱色谱分离、浓缩和真空干燥提取制备,通过对柱色谱分离条件的实验分析,找到最佳控制条件:用聚酰胺树脂对儿茶素进行分离纯化,最佳洗脱顺序为25%乙醇,乙酸乙酯:80%乙醇=2:1,生产出低乙酸乙酯的儿茶素。产品质量指标为:乙酸乙酯低于国际标准20mg/kg,儿茶素≥75%,EGCG≥55%,咖啡因<2%,收率>10%。      

儿茶素和表儿茶素异构体的高效逆流色谱分离制备

应用高效逆流色谱法(HPCCC)对茶叶中的儿茶素和表儿茶素两种同分异构体的分离制备方法进行研究。结果表明：以正己烷-乙酸乙酯-水(体积比1:20:20)为两相溶剂系统,上相为固定相,下相为流动相,可以实现儿茶素和表儿茶素的完全分离。采用138mL的分离柱、1g儿茶素粗提物,在120min内一次制备即可得到纯度在95%以上的表儿茶素约35mg,纯度在99%以上的儿茶素325mg,纯度90%～99%的儿茶素100mg。     

儿茶素单体分离制备方法

茶叶中含有丰富的儿茶素类物质,占茶叶干重12%～24%,是茶叶中最具生理活性和保健功效的物质。文中对目前国内外纯化制备儿茶素的常见方法进行了综述。常见的儿茶素制备方法包括纤维素柱层析、葡聚糖凝胶(Sephadex LH—20)、硅胶柱层析、吸附树脂柱层析和高速逆流色谱等方法。通过这些方法制备的儿茶素单体纯度不高,仍需结合结晶、制备型液相色谱技术或膜分离技术进行进一步纯化,从而才能获得高纯度的儿茶素单体。在儿茶素单体的制备方法中,每种方法都有相应的优缺点。Sephadex LH—20柱层析分离的量较大,但是分离时间较长,而且Sephadex LH—20柱填料昂贵;高速逆流色谱分离效果较好,得到的儿茶素单体的纯度较高,分离时间相对要短,但是目前市场上只有分析型,分离的量相对少;硅胶材料廉价,但是分离的效果不佳,且分离过程相对繁琐,单体制备量较小;吸附树脂柱层析分离已实现EGCG单体的工业化生产,但在其他儿茶素单体的分离制备上尚不成熟。     

高速逆流色谱法分离制备柿子中儿茶素及表儿茶素

采用HP2MGL大孔树脂对柿子中的儿茶素类物质进行初步分离,用高速逆流色谱进一步分离纯化柿子中的(-)-儿茶素、(-)-表儿茶素。结果表明,在以正丁醇-乙酸乙酯-水(体积比为1:2:3)组成的溶剂体系,上相为固定相,下相为流动相,转速800r/min,流速1mL/min的条件下进行HSCCC制备,经高效液相法测定,从58mg样品中分离出7.25mg(-)-儿茶素和0.43mg(-)-表儿茶素,纯度分别为98.3%和97.9%。     

茶叶儿茶素单体的分离纯化及鉴定

将茶提取物（茶多酚）先经SephadexLH-20柱层析分离,脱除咖啡因和色素,并将其中7种儿茶素分成2个流分.再用半制备型HPLC分离纯化,得到7种儿茶素的单体化合物.用UV、IR、NMR及MS等方法鉴定和验证了其化学结构,7种单体儿茶素化合物的纯度均大于99%,总得率为66.7%,总回收率为82.1%.     

制备高纯L-表没食子儿茶素没食子酸酯的工艺优化研究

选择聚酰胺为柱填料,以商品茶多酚为原料,考察了溶剂的不同比例、洗脱剂pH值、温度、流速等对纯化分离L-表没食子儿茶素没食子酸酯(-)-EGCG)影响.获得的工艺条件是:在玻璃层析柱(500 mm ×20 mm)中,装填聚酰胺(粒径150～75μm)树脂,上样量为42.9mgTP/g树脂,用洗脱剂(甲醇:水=4:1),pH3.5～4.5,温度为室温(或25℃),流速为4.0mL/min的情况下洗脱,可以得到(-)-EGCG的纯度达93%以上.     

表没食子儿茶素没食子酸酯的抗癌机制的研究进展

表没食子儿茶素没食子酸酯(epigallocatechin gallate,EGCG)是茶叶中主要的活性成分之一,具有抗氧化、抗炎症、抗癌等生理功效。在癌症的治疗和预防研究中,研究者将EGCG作为一种高效的天然化学预防剂,并期望将EGCG开发为保健食品和药品。本文就近年来国内外对EGCG抗癌活性、抗癌机理(抗氧化、抑制血管生成、诱导癌细胞周期阻滞、诱导癌细胞凋亡、抗炎症)方面的研究工作进行概述;并就当前EGCG在抗癌方面存在的缺陷提出解决方案和可实行的改进技术措施。      

茶树花多酚儿茶素单体分离纯化研究

茶树花多酚样品先经葡聚糖凝胶Sephadex LH-20柱层析预分离,脱除咖啡碱等杂质,并将儿茶素分为八个流分,再用硅胶柱分离纯化,得到四种儿茶素的单体化合物。HPLC测定四种单体儿茶素化合物的纯度,EC纯度98.9%、ECG纯度96.8%、EGCG纯度98.6%、GCG纯度97.1%。     

中低压C18柱层析分离儿茶素单体的研究

本文采用中低压柱层析制备色谱仪,研究了AB-8大孔吸附树脂、C18、聚酰胺树脂、硅胶4种不同柱层析吸附材料对茶多酚的分离效果,最终选择C18作为最佳层析材料,考察了不同的茶多酚进样量、流速对儿茶素分离效率的影响。结果表明以C18作为柱层析材料,甲醇水溶液进行梯度洗脱,可得到EGCG、GCG、ECG、CG四种儿茶素,其最高总得率为68.44%,且确定最佳工艺条件:350mg茶多酚进样量在20mL/min流速下进行甲醇水溶液梯度洗脱,可获到EGCG,GCG,ECG,CG四种儿茶素,其得率分别为36.19%±0.11%、7.42%±0.14%、12.93%±0.18%、2.40%±0.22%,而其纯度分别为88.85%±0.17%、83.74%±0.09%、96.01%±0.13%、70.67%±0.11%。该工艺操作简单,纯化分离效果较好;可为进行规模化、工业化生产提供参考。     

利用活性真菌转化简单儿茶素为酯型儿茶素

研究从茶树的鲜叶、茎部和茶树土壤中分离出活性真菌,通过利用天然微生物的转化能力,使简单儿茶素转化为功能性较强的复杂型酯型儿茶素。实验结果表明:筛选出了具有转化能力的活性菌种,能有效地将简单儿茶素转化为酯型儿茶素,而且其转化能力良好。并对此种活性真菌进行形态学和生理生化的初步检测,判断其属于丝状真菌藻状菌纲,毛霉目,内囊霉科,内囊霉属。     

Analysis of tea catechins in vegetable oils by high‐performance liquid chromatography combined with liquid–liquid extraction

In this study, a method was developed for the determination of various tea catechins in vegetable oils. Firstly, vegetable oils including tea seed oil, sunflower seed oil and soya bean oil were extracted by methanol/water (40:60, v/v), and then, a high‐performance liquid chromatography (HPLC) method was developed for the simultaneous determination of GA, caffeine, EGC, EGCG, EC, ECG, GC, GCG, C and CG. For the compounds detected in tested vegetable oils, LODs were in the range of 0.05–1.65 ng, both intraday and interday relative standard deviations (RSDs) were <5.0%, and the recovery rates were in the range of 96.2–100.5% with RSD <3.7%. The results showed in vegetable oils which declared to had added tea catechins in, the concentrations of tea catechins were less than that showed in package label, and the content of EGCG was the highest in all samples. Therefore, the advancement made in our study will facilitate studies of tea catechins in oil industry.     

Analysis of some selected catechins and caffeine in green tea by high performance liquid chromatography

Green tea seems to have a positive impact on health due to the catechins-found as flavanols. Thus, the present study was aimed to develop a low cost reversed phase high performance liquid chromatographic (HPLC) method for simultaneous determination of flavanol contents, namely catechin (C), epicatechin (EC), epigallocatechin (EGC), epicatechin 3-gallate (ECG) and epigallocatechin 3-gallate (EGCG) and caffeine in 29 commercial green tea samples available in a Saudi Arabian local market. A C-18 reversed-phase column, acetonitrile–trifluoroacetic acid as a mobile phase, coupled with UV detector at 205 nm, was successfully used for precise analysis of the tested analytes in boiled water of digested tea leaves. The average values of N (No. of theoretical plates), HETP (height equivalent of theoretical plates) and R_s (separation factor) (at 10 μg ml⁻¹ of the catechins EC, EGC, EGCG and ECG) were 2.6 × 10³ ± 1.2 × 10³, 1.7 × 10⁻³ ± 4.7 × 10⁻⁴ cm and 1.7 ± 5.53 × 10⁻², respectively. The developed HPLC method demonstrated excellent performance, with low limits of detection (LOD) and quantification (LOQ) of the tested catechins of 0.004–0.05 μg ml⁻¹ and 0.01–0.17 μg ml⁻¹, respectively, and recovery percentages of 96–101%. The influence of infusion time (5–30 min) and temperature on the content of the flavanols was investigated by HPLC. After a 5 min infusion of the tea leaves, the average concentrations of caffeine, catechin, EC, EGC, ECG and EGCG were found to be in the ranges 0.086–2.23, 0.113–2.94, 0.58–10.22, 0.19–24.9, 0.22–13.9 and 1.01–43.3 mg g⁻¹, respectively. The contents of caffeine and catechins followed the sequence: EGCG > EGC > ECG > EC > C > caffeine. The method was applied satisfactorily for the analysis of (+)-catechin, even at trace and ultra trace concentrations of catechins. The method was rapid, accurate, reproducible and ideal for routine analysis.     

Epimerisation and hydrolysis of catechins under ultrasonic treatment

This study investigated the influence of ultrasonic treatments on the chemical conversions of catechins. Ultrasound treatments significantly enhanced the epimerisation and the hydrolysis of catechins in both the catechins solution and the tea extract solution. Catechins are more stable in the tea extract solution compared to the catechins solution. The conversion of catechins induced by ultrasound can be controlled by temperature and pH. Regard to the pyrogallol-type catechins, both the epimerisation and the hydrolysis were enhanced at the higher temperatures (60 and 70 °C) and the acidic condition (pH 6). The epimerisation and the hydrolysis of (-)-epigallocatechin gallate (EGCG) improved by 47% and 18%, respectively, when the temperature rose from 50 to 70 °C. Compared to pH 8, the epimerisation and the hydrolysis of EGCG at pH 6 improved by 27% and 39%, respectively. This study can be utilised to develop appropriate ultrasound-assisted method to produce particular catechin monomers.     

儿茶素的药理作用研究综述

对儿茶素及其类似化合物所具有的抗氧化、保护心血管、抗肿瘤、抗菌、抗病毒、抗炎、免疫调节、神经保护、调节糖脂代谢等药理作用进行了综述,指出其具有重要的医疗保健应用价值,儿茶素类的手性研究及其体内与金属离子、蛋白质等物质的相互作用将是今后研究开发的重点.     

Comparison of catechins and aromas among different green teas using HPLC/SPME-GC

Green tea polyphenols (GTP) from Camellia sinensis (L.) O. Kuntze are the major water soluble components in tea liquor. The GTP extraction yield was determined using different extraction times from 10 to 60 min at 70°C, and also at different temperatures from 50°C to 100°C, keeping the extraction time constant. The composition of the GTP (catechins) from samples of different origins was determined by RP–HPLC, measuring the absorbance at 280 nm. The calibration curves of the catechins were linear between 5 ng and 2 μg, and their C.V. values for the quantitation were less than 4.0% for four replicates using four different sets of each type. The total epicatechin derivatives (EPD) and epigallocatechin-3-gallate (EGCG) from Azorean green tea, accounted for 74.5 and 47.9% (w/w) of the total GTP, respectively, and were compared with that from tea samples of different origins. The EGCG:caffeine ratio in Azorean green tea was fourfold higher as compared with others, which suggested a good source of a chemopreventive agent. The aroma composition of different green tea samples was compared using the SPME/GC headspace methodology.     

The roles of catechins and caffeine in cream formation in a semi-fermented tea

The mechanism of cream formation in a semi-fermented tea was investigated by adding caffeine or catechins to the de-creamed tea infusions. The addition of catechins to the clarified infusion could not re-induce cream formation. However, creaming occurred again after replenishing the de-creamed tea infusion with caffeine. It was thought that the ester-form catechins which possessed a galloyl group and a hydroxylphenyl B ring acted like a claw. They could thus entrap and interact with caffeine more effectively through hydrogen bonding and hydrophobic interaction to form a large complex, resulting in creaming. © 1999 Society of Chemical Industry     

气相色谱法测定酱油中乙酸乙酯的含量

乙酸乙酯是酱油中的香气成分之一,其含量虽不多,但对酱油的香气有举足轻重的影响.文章采用顶空气相色谱法测定酱油中的乙酸乙酯含量,避免了对色谱柱和检测器的污染,免除了蒸馏的步骤.结果显示,在所测定的酱油样品中乙酸乙酯的含量在2.32 μg/mL和36.3 μg/mL之间,方法的回收率为91.93%～97.25%,相对标准偏差为1.2%,能满足酱油中微量成分的分析.     

儿茶素稳态化及其应用研究进展

儿茶素是茶叶主要的品质与功能化学成分,具有多种生理功能。但儿茶素不稳定,在实际应用中存在一定的局限性。本文对影响儿茶素稳定性的因素以及儿茶素稳态化的技术和应用进行综述,为儿茶素的相关研究及综合应用提供理论参考。      

儿茶素类的保健作用及机制

茶是二十一世纪风靡全球的健康饮料。茶叶中含有多种保健功能成分, 尤其是儿茶素类物质。儿茶素 具有诸多医疗保健功能和一些特殊性质, 不仅被应用于经口服的膳食补充剂、保健食品、保健饮料等产品, 还应用于化妆品、日化用品等外用型的健康产品, 具有良好的市场开发潜力。本文综述了内服和外用两种方式下儿茶素类物质的保健作用及其作用机制。