Phenolic,Carotenoid and Saccharide Compositions of Vietnamese Camellia sinensis Teas and Herbal Teas

Tea (Camellia sinensis) and herbal tea have been recognized as rich sources of bioactive constituents with the ability to exert antioxidant actions. The aims of this study were to analyze phenolic, carotenoid and saccharide contents in a set of Vietnamese tea and herbal tea and compare the results with those of green and black teas marketed in the U.S. In total, 27 phenolics, six carotenoids and chlorophylls, and three saccharides were quantitatively identified. Catechins, quercetin glycosides and chlorogenic acid were the predominating phenolics in the teas, with the concentrations following the order: jasmine/green teas > oolong tea > black tea. Lutein was the dominant carotenoid in the teas and its concentrations were generally found to be higher in the jasmine and green teas than in the oolong and black teas. The study showed that the green teas originating in Vietnam had much higher levels of phenolics and carotenoids than their counterparts stemming from another country. The application of partial least squares discriminant analysis (PLS-DA) as a chemometric tool was able to differentiate phenolic profiles between methanolic extracts and tea infusions. Through principal component analysis (PCA), the similarities and dissimilarities among the jasmine, green, oolong, black teas and herbal teas were depicted.     

Effects of different steeping methods and storage on caffeine, catechins and gallic acid in bag tea infusions

Bag teas, packed 3g of ground black, green, oolong, paochoung and pu-erh tea leaves (the particle size used was 1-2mm), were steeped in 150 mL of 70, 85 or 100 degrees C hot water to study the effects of the number of steeping (the same bag tea was steeped repeatedly eight times, 30s each time, as done in China for making ceremonial tea) and varied steeping durations (0.5-4 min) on caffeine, catechins and gallic acid in tea infusions. The changes in tea infusions during storage at 4 or 25 degrees C for 0-48 h and the variations in these compounds of bag tea infused with 150 mL of 4 or 25 degrees C cold water for 0.5-16 h were also investigated. A HPLC method with a C18 column and a step gradient solvent system consisting of acetonitrile and 0.9% acetic acid in deionized water was used for analysis. Results for all kinds of tea samples showed that the second tea infusion contained the highest contents of caffeine, catechins and gallic acid when bag teas were steeped in 70 degrees C water. It was different from that steeped at 85 and 100 degrees C, the highest contents existed in the first infusion. These compounds decreased gradually in later infusions. Higher amounts of caffeine, catechins and gallic acid could be released from bag teas as hotter water was used. As steeping duration prolonged, these ingredients increased progressively, however, their levels were lower than that cumulated from the infusions with the identical bag tea prepared recurrently at the same temperature and time points. (-)-Gallocatechin gallate and (+)-catechin existed in these tea infusions rarely and could not be detected until a certain amount of them infusing. Except gallic acid that showed a significant increase and caffeine that exhibited no significant change, all kinds of catechins decreased appreciably after tea infusions were stored at 25 degrees C for 36 h; nevertheless, all of them showed no evident changes at 4 degrees C storage. The caffeine, catechins and gallic acid in tea infused with cold water also increased with increasing duration. Their contents in 25 degrees C steeped tea were higher than that made at 4 degrees C; moreover, their infusion rates from bag teas to cold water were markedly lower than that steeped in hot water. Infusing efficiencies of non-gallated catechins were higher than gallated catechins under cold water steeping.     

GC-MS法快速测定茶叶中脂肪酸

建立了气相色谱-质谱联用技术(GC-MS)快速分析茶叶脂肪酸的新方法.对23批茶叶样品进行GC-MS分析,结合NIST 05谱库检索鉴定茶叶脂肪酸种类,并用峰面积归一化法测定其相对含量,比较不同加工方式的茶叶脂肪酸含量.结果表明,所有茶样中亚麻酸、亚油酸和棕榈酸含量最高,但绿茶和青茶脂肪酸含量高于发酵处理的红茶和黑茶.方法可以用于分析各种茶叶的脂肪酸,反映不同种类茶叶的性质差异.     

Simultaneous determination of catechins, caffeine and gallic acids in green, Oolong, black and pu-erh teas using HPLC with a photodiode array detector

A simple and fast HPLC method using a photodiode array detector was developed for simultaneous determination of four major catechins, gallic acid and caffeine. After multiple extractions with aqueous methanol and acidic methanol solutions, tea extract was separated within 20 min using a methanol-acetate-water buffer gradient elution system on a C(18) column. The sample extraction data demonstrated that the single extraction used in the previous studies with aqueous acetonitrile or methanol is not sufficient; the multiple extraction procedure is essential for the quantitative analysis of catechins, phenolic acids and caffeine in teas. Several green, Oolong, black and pu-erh teas were successfully analyzed by this method. The analytical results obtained indicated that green teas contain higher content of catechins [(-)-epigallocatechin gallate, (-)-epigallocatechin, (-)-epicatechin gallate, and (-)-epicatechin] than both Oolong, pu-erh and black teas because fermentation process during the tea manufacturing reduced the levels of catechins significantly. The fermentation process also remarkably elevated the levels of gallic acid in full-fermented pu-erh and black teas. Another interesting finding is the low level of caffeine in Oolong teas, especially in Fujian Oolong tea.     

Simple and rapid UV spectrophotometry of caffeine in tea coupled with sample pre-treatment using a cartridge column filled with polyvinylpolypyrrolidone (PVPP)

We have applied a sample pre-treatment method with a cartridge column filled with polyvinylpolypyrrolidone (PVPP) to the effective removal of polyphenols and simple UV spectrophotometry of caffeine in tea. The absorption maximum length (lambda(max)) for caffeine was close to those for tea catechins in aqueous 1% acetic acid; therefore, the UV spectrum of a non-treated green tea sample had a large absorption wave. In contrast, the absorbance of the green tea sample was gradually reduced by PVPP cartridge treatment using PVPP from 0 to 50 mg, and was nearly constant using a pre-treatment cartridge with more than 100 mg PVPP, because tea catechins were effectively removed and caffeine was mostly recovered from a green tea sample by means of PVPP cartridge treatment. The PVPP pre-treatment cartridge also removed polyphenols successfully from oolong and black tea samples. Comparison with conventional HPLC analysis indicated that the present pre-treatment method with a PVPP cartridge was useful for the simple and selective UV spectrophotometric determination of caffeine in green, oolong and black tea samples.     

Determination of Pesticide Residues in Teas via QuEChERS Combined with Dispersive Liquid–Liquid Microextraction Followed by Gas Chromatography–Tandem Mass Spectrometry

In this study, an effective gas chromatography–tandem mass spectrometry method was developed to determine 47 pesticide residues in tea. Sample preparation involved a quick, easy, cheap, effective, rugged, and safe (QuEChERS) procedure, wherein the sample is extracted by acetonitrile and cleaned up with multiwalled carbon nanotubes and primary secondary amine adsorbents; dispersive liquid–liquid microextraction (DLLME) was subsequently performed using carbon tetrachloride as extractive solvent and the extract obtained by QuEChERS as dispersive solvent. Factors influencing DLLME efficiency, including type and volume of extractive solvent, volume of dispersive solvent, and extraction time were evaluated. For validation purposes, recovery studies were performed using matrix blanks fortified with pesticides at three concentrations, namely, 10, 50, and 100 μg kg^?1. Most of the analytes were recovered at an acceptable range of 70?120% and RSDs ≤ 20% were acquired for green tea, oolong tea, black tea, and puer tea. Limits of quantification of pesticides obtained for these teas were sufficiently low, and most pesticides levels were lower than 10 μg kg^?1, which satisfies the requirements for maximum residue levels (MRLs) as prescribed by the European Community. Twenty-four commercially available tea samples were analyzed using this optimized method. Results revealed that the contents of chlorpyrifos and alpha-HCH from different green tea samples exceed the MRLs, and chlorpyrifos, bifenthrin, lambda-cyhalothrin, and cypermethrin are among the most frequently detected pesticides in teas.     

Improved sample pre-treatment for determination of caffeine in tea using a cartridge filled with polyvinylpolypyrroridone (PVPP)

We have improved sample pre-treatment for the effective removal of polyphenols and simple analysis of caffeine in tea using a cartridge filled with polyvinylpolypyrroridone (PVPP). Nearly 100% of catechins were removed from the green tea sample and caffeine was completely recovered in the range of 98.2-101.3% by sample pre-treatment with a PVPP cartridge. Reproducibility of preparing PVPP pre-treatment cartridges was sufficient for quantitative analysis, because RSDs of analytical values for caffeine obtained by using three individual pre-treatment cartridges filled with 10-200 mg PVPP were 0.60-2.8%. The PVPP pre-treatment cartridge also removed polyphenols perfectly and recovered caffeine faultlessly from oolong and black tea samples. Comparison with the conventional method without sample pre-treatment indicated that the present pre-treatment method with a PVPP cartridge was useful for the simple and precise analysis of caffeine in green, oolong and black tea samples.     

Identification of Key Aroma Compounds Responsible for the Floral Ascents of Green and Black Teas from Different Tea Cultivars

Chemicals underlying the floral aroma of dry teas needs multi-dimensional investigations. Green, black, and freeze-dried tea samples were produced from five tea cultivars, and only ‘Chunyu2’ and ‘Jinguanyin’ dry teas had floral scents. ‘Chunyu2’ green tea contained the highest content of total volatiles (134.75 μg/g) among green tea samples, while ‘Jinguanyin’ black tea contained the highest content of total volatiles (1908.05 μg/g) among black tea samples. The principal component analysis study showed that ‘Chunyu2’ and ‘Jinguanyin’ green teas and ‘Chunyu2’ black tea were characterized by the abundant presence of certain alcohols with floral aroma, while ‘Jinguanyin’ black tea was discriminated due to the high levels of certain alcohols, esters, and aldehydes. A total of 27 shared volatiles were present in different tea samples, and the contents of 7 floral odorants in dry teas had correlations with those in fresh tea leaves (p < 0.05). Thus, the tea cultivar is crucial to the floral scent of dry tea, and these seven volatiles could be promising breeding indices.     

Widely Targeted Metabolomics Analysis Reveals Great Changes in Nonvolatile Metabolites of Oolong Teas during Long-Term Storage

As a semifermented tea, oolong is exceedingly popular worldwide for its elegant, flowery aroma and mellow, rich taste. However, recent marketing trends for old oolong teas and their chemical quality largely remain unexplored. In this study, we applied widely targeted metabolomics using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) combined with multivariate analysis to investigate the chemical change of oolong teas in the aging process. With the increasing of store time, most nongalloylated catechins; tannins, including TFs and proanthocyanidins; flavonols and glycosylated flavonols; amino acids and their derivatives; nucleotides and their derivatives; and lots of alkaloids and phospholipids declined, while most fatty acids and organic acids increased, and galloylated catechins, GA, and caffeine were almost stable. The result also suggested that approximately seven years (but not an infinite extension) was a special period for oolong tea storage, which brings about excellent taste.     

Chromatographic Determination of the Mycotoxin Patulin in 219 Chinese Tea Samples and Implications for Human Health

Patulin (PAT) is a mycotoxin, with several acute, chronic, and cellular level toxic effects, produced by various fungi. A limit for PAT in food of has been set by authorities to guarantee food safety. Research on PAT in tea has been very limited although tea is the second largest beverage in the world. In this paper, HPLC−DAD and GC−MS methods for analysis of PAT in different tea products, such as non-fermented (green tea), partially fermented (oolong tea, white tea, yellow tea), completely fermented (black tea), and post-fermented (dark tea and Pu-erh tea) teas were developed. The methods showed good selectivity with regard to tea pigments and 5-hydroxymethylfurfural (5-HMF) and a recovery of 90–102% for PAT at a 10–100 ppb spiking level. Limit of detection (LOD) and limit of quantification (LOQ) in tea were 1.5 ng/g and 5.0 ng/g for HPLC−UV, and 0.25 ng/g and 0.83 ng/g for GC−MS. HPLC was simpler and more robust, while GC−MS showed higher sensitivity and selectivity. GC−MS was used to validate the HPLC−UV method and prove its accuracy. The PAT content of 219 Chinese tea samples was investigated. Most tea samples contained less than 10 ng/g, ten more than 10 ng/g and two more than 50 ng/g. The results imply that tea products in China are safe with regard to their PAT content. Even an extreme daily consumption of 25 g of the tea with the highest PAT content (124 ng/g), translates to an intake of only 3 μg/person/day, which is still an order of magnitude below the maximum allowed daily intake of 30 µg for an adult.     

Removal of caffeine from green tea by microwave-enhanced vacuum ice water extraction

In order to selectively remove caffeine from green tea, a microwave-enhanced vacuum ice water extraction (MVIE) method was proposed. The effects of MVIE variables including extraction time, microwave power, and solvent to solid radio on the removal yield of caffeine and the loss of total phenolics (TP) from green tea were investigated. The optimized conditions were as follows: solvent (mL) to solid (g) ratio was 10:1, microwave extraction time was 6 min, microwave power was 350 W and 2.5 h of vacuum ice water extraction. The removal yield of caffeine by MVIE was 87.6%, which was significantly higher than that by hot water extraction, indicating a significant improvement of removal efficiency. Moreover, the loss of TP of green tea in the proposed method was much lower than that in the hot water extraction. After decaffeination by MVIE, the removal yield of TP tea was 36.2%, and the content of TP in green tea was still higher than 170 mg g⁻¹. Therefore, the proposed microwave-enhanced vacuum ice water extraction was selective, more efficient for the removal of caffeine. The main phenolic compounds of green tea were also determined, and the results indicated that the contents of several catechins were almost not changed in MVIE. This study suggests that MVIE is a new and good alternative for the removal of caffeine from green tea, with a great potential for industrial application.     

Quasi-flow injection analysis for rapid determination of caffeine in tea using the sample pre-treatment method with a cartridge column filled with polyvinylpolypyrrolidone

The sample pre-treatment method using a polyvinylpolypyrrolidone (PVPP) cartridge column combined with a quasi-flow injection analysis (quasi-FIA) system realized the rapid determination of caffeine in three types of tea, green, oolong and black tea. The measurement time for each tea sample pre-treated using a PVPP cartridge column was shortened to 20s. In the present system, the limits of detection and quantification were 0.3 microM (1.5 pmol injected) and 0.7 microM (3.5 pmol injected), respectively, and a linear calibration curve was afforded up to 800 microM (4 nmol injected). Within-run precision of analysis of standard solutions of 10 and 100 microM caffeine was 0.11 and 0.16% (n=6), respectively. Between-run precision of analysis of the same solutions over 6 days was 0.78 and 0.74% (n=6), respectively. Comparison with the conventional HPLC method indicated that the present quasi-FIA method using sample pre-treatment with a PVPP cartridge column was useful for the simple and precise determination of caffeine in green, oolong and black tea samples.     

Influence of Tea Brewing Parameters on the Antioxidant Potential of Infusions and Extracts Depending on the Degree of Processing of the Leaves of Camellia sinensis

The polyphenol content of tea depends on the growing region, harvest date, the production process used, and the brewing parameters. In this study, research was undertaken that included an analysis of the influence of the brewing process parameters on the content of total polyphenols (Folin-Ciocalteu), epigallocatechin gallate (HPLC), and antioxidant activity (against DPPH radicals) of fresh tea shrub leaves grown from Taiwan and of teas obtained from them (oolong, green in bags, and green loose from the spring and autumn harvest). The antioxidant potential was determined in the methanol and aqueous extracts, as well as in infusions that were obtained by using water at 65 or 100 °C and infusing the tea for 5 or 10 min. The highest content of total polyphenols and epigallocatechin gallate was found in green tea extracts from the spring harvest. However, in the case of infusions, the highest content of these compounds was found in green tea in bags. Steaming at 100 °C for 10 min, turned out to be the most favourable condition for the extraction. Oolong tea, brewed at 100 °C for 5 min was characterised by the highest antioxidant activity against stable DPPH radicals.     

Evaluation of ice‐tea quality by DART‐TOF/MS

DART (Direct Analysis in Real Time) coupled with Time‐of‐Flight Mass Spectrometry (TOF/MS) has been used for analyses of ice‐teas. The article focuses on quality and authenticity of ice‐teas as one of the most important tea‐based products on the market. Twenty‐one samples of ice‐teas (black and green) were analysed. Selected compounds of ice‐teas were determined: theobromine, caffeine, total phenolic compounds, total soluble solids, total amino acid concentration, preservatives and saccharides were determined. Fingerprints of DART‐TOF/MS spectra were used for comprehensive assessment of the ice‐tea samples. The DART‐TOF/MS method was used for monitoring the following compounds: citric acid, caffeine, saccharides, artificial sweeteners (saccharin, acesulphame K), and preservatives (sorbic and benzoic acid), phosphoric acid and phenolic compounds. The measured data were subjected to a principal components analysis. The HPLC and DART‐TOF/MS methods were compared in terms of determination of selected compounds (caffeine, benzoic acid, sorbic acid and saccharides) in the ice‐teas. The DART‐TOF/MS technique seems to be a suitable method for fast screening, testing quality and authenticity of tea‐based products. Copyright © 2015 John Wiley & Sons, Ltd.     

Classificatin of chinese tea samples according to origin and quality by principal component techniques

Three categories of tea, black, green and oolong tea, with those varieties in each category were analyzed for their contents of cellulose, hemicellulose, lignin, polyphenols, caffeine and amino acids. The data were subjected to multivarige analysis. Principal component analysis and principal component classification provide discrimination between the different categories and varieties. The quality index, assigned to these tea standards by experts, could be predicted form the principal component scores.     

Quantification of Antioxidant Properties in Popular Leaf and Bottled Tea by High-performance Liquid Chromatography (HPLC), Spectrophotometry,and Voltammetry

Polyphenols in plants such as tea may offer many health benefits. The leaf and bottled teas available on the market today are advertised with a strong emphasis on their antioxidant properties. In this study, we have quantified the total polyphenol, flavonoid, and theaflavin concentrations by simple colorimetric methods, measured the reactivity of polyphenols using direct and indirect oxidation methods, and identified specific polyphenols present using high-performance liquid chromatography in a variety of commercially available teas. We find that, per given volume, freshly brewed teas are richer in polyphenols and reactivity by a factor five or more compared to bottled teas. Within the brewed and bottled categories, white and green teas are richer in antioxidants than oolong and black teas although the differences are less than a factor of two. We also find that the presence of additives causes changes in antioxidant properties such as an enhancement in Cranberry Orange tea and a reduction in Earl Grey tea. Since we verified our results using several overlapping techniques, we are able to evaluate the analytical tools commonly used in antioxidant studies. We find that the Folin–Ciocalteu method of quantifying polyphenols is a good indicator of the relative antioxidant reactivity of teas.     

Analytical separation of tea catechins and food-related polyphenols by high-speed counter-current chromatography

High-speed counter-current chromatography (HSCCC) using the type-J coil planet centrifuge was applied to compositional analysis of tea catechins and separation of other food-related polyphenols. The HSCCC separation of nine different standard compounds and those from extracts of commercial tea leaves was performed with a two-phase solvent system composed of tert-butyl methyl ether-acetonitrile-0.1% aqueous trifluoroacetic acid (TFA) (2:2:3, v/v/v) by eluting the upper organic phase at a flow rate of 2 ml/min. The main compounds in the extract of non-fermented green tea were found to be monomeric catechins, their galloylated esters and caffeine. In addition to these compounds, oxidized pigments, such as hydrophobic theaflavins (TFs) and polar thearubigins (TRs) were also separated and detected from the extracts of semi-fermented oolong tea and fermented black tea. Furthermore, several food-related polyphenols, such as condensed catechin oligomers (procyanidins), phenolic acids and flavonol glycosides were clearly separated under the same HSCCC condition. These separation profiles of HSCCC provide useful information about the hydrophobic diversity of these bioactive polyphenols present in various types of teas and food products.     

Fast and simultaneous determination of phenolic compounds and caffeine in teas, mate, instant coffee, soft drink and energetic drink by high-performance liquid chromatography using a fused-core column

A fast HPLC method with diode-array absorbance detector and fluorescence detector for the analysis of 19 phenolic acids, flavan-3-ols, flavones, flavonols and caffeine in different types of samples was developed. Using a C₁₈ reverse-phase fused-core column separation of all compounds was achieved in less than 5 min with an overall sample-to-sample time of 10 min. Evaluation of chromatographic performance revealed excellent reproducibility, resolution, selectivity and peak symmetry. Limits of detection for all analyzed compounds ranged from 0.5 to 211 μg L⁻¹, while limits of quantitation ranged between 1.5 and 704 μg L⁻¹. The developed method was used for the determination of analytes present in different samples, including teas (black, white, green), mate, coffee, cola soft drink and an energetic drink. Concentration of the analyzed compounds occurring in the samples ranged from 0.4 to 314 mg L⁻¹. Caffeine was the analyte found in higher concentrations in all samples. Phytochemical profiles of the samples were consistent with those reported in the literature.     

Dynamic ultrasound-assisted extraction of catechins and caffeine in some tea samples

A novel dynamic ultrasound-assisted extraction (DUAE) device has been constructed for extraction of five catechins and caffeine in solid sample. The accurate, simple, reproducible and sensitive method for the determination of five catechins and caffeine has been developed and validated. A comparison has been made of the efficiencies by employing DUAE and conventionally static ultrasound-assisted extraction (UAE). The proposed method can not only improve extraction efficiency but also decrease time and solvent consumption. The commercial Chinese tea samples, involving green and black teas, are rapidly analyzed by the proposed DUAE method. The linearity, range, selectivity, precision, accuracy, and robustness also showed acceptable values.