A kind of preparation method of Yunnan black tea extract and application thereof
Technical field:
The present invention relates to the extraction and the application of tealeaves in the natural perfume material, be specifically related to a kind of preparation method and application thereof of Yunnan black tea extract.
Background technology:
China is the native place of tealeaves, is to find and utilize tealeaves country the earliest.Tealeaves has multiple efficacies such as medicinal, edible.Tea extract contains amino acid and multiple active skull cap components; Like polyphenol, catechin, polysaccharide, vitamin, alkaloid etc.; Have the functions such as benefit think of, permanent tooth preventing decayed tooth, antiphlogistic and bactericidal, the anticancer change of radiation proof of refreshing oneself; And side effect is little, is a kind of broad-spectrum natural plant extracts, and is extensive in sector applications such as food, beverage, cosmetics.
Yunnan black tea tea is a kind of of China's six big teas; Its extract is a kind of traditional tobacco charging raw material, and it has the effect that lasting is lasting, improve cigarette odor-absorbing and flavouring essence quality.At present domestic most employing low-concentration ethanol continuous extraction legal system is equipped with tea extract, but this method has two big shortcomings: 1. the leaching process time longer, be prone to make part natural tea fragrance loss; 2. in the product except that fragrance component, also contain some protein, impurity component, dissolubility is bad, makes product when using, receive certain restriction.Therefore, how to extract the effective fragrance component in the black tea effectively, and improve its fragrance content, improve the black tea extract quality, make it can obtain more perfect utilization, become the development trend of tealeaves spices.
Summary of the invention:
The purpose of this invention is to provide a kind of preparation method and application thereof of Yunnan black tea extract, utilize Extraction by Ultrasound Yunnan black tea tea can improve the yield of Yunnan black tea extract, the binding silica gel chromatography has improved the quality and the purity of active ingredient; And then the interior quality of raising cigarette.
The objective of the invention is to realize through following proposal, is raw material with Yunnan black tea tea, uses mixed solvent, ultrasonic extraction method to obtain, and wherein the preparation method of Yunnan black tea extract prepares through following steps:
Step 1: in the Extraction by Ultrasound jar, add Yunnan black tea tea, add mixed solvent, opening device, temperature remains under 60-70 ℃, extracts 30-60 minute, stops operation, and pours out extract after the cooling slightly, uses strainer filtering, collects extract; Recrement continues to carry out the second time with said method and extracts, and filters and collects extract for the second time;
Step 2: merge extracted twice liquid, on rotary evaporator, concentrate, thickening temperature 60-90 ℃, vacuum 0.03-0.1Mpa;
Step 3: the ethyl acetate mixed processing that benzinum that to be 1.0 ± 0.02 concentrate with the proportion that obtains doubly measure with 0.5-2 and 2-5 doubly measure, remove insoluble matter, and reclaim solvent;
Step 4: the concentrate after the step 3 processing is placed on the silica gel column chromatography, as solvent, carry out chromatography, behind the recovery solvent, obtain Yunnan black tea extract with benzinum.
The preparation method of above-mentioned Yunnan black tea extract, described concentrate content is: Polyphenols 4-16%, catechin 5-10%, amino acids 0.5-3.0%, carbohydrate 2.0-10%, alkaloid 1-8.0%.
The preparation method of above-mentioned Yunnan black tea extract, described mixed solvent is made up of ethanol, propane diols, water, citric acid.
The preparation method of above-mentioned Yunnan black tea extract, said Yunnan black tea tea raw material is the tealeaves of fermentation, moisture is at 7-20%.
The preparation method of above-mentioned Yunnan black tea extract, solid-liquid ratio is 1 in the described ultrasonic Treatment: 8-1: 20, ultrasonic power is 15-60kHz, extraction time is 30-60min.
Above-mentioned Yunnan black tea extract, the appearance characteristics of said extract is yellow green or dark brown.
A kind of application of Yunnan black tea extract takes by weighing Yunnan black tea extract by the 0.01-0.05% of cigarette shreds, uses 60% dissolve with ethanol, and spray is added in the flue-cured tobacco pipe tobacco, is rolled into the cigarette finished product.
The invention has the advantages that: compare with conventional method of extraction, use the Yunnan black tea tea of mixed solvent, Extraction by Ultrasound, greatly reduce consumption of ethanol, reduce and extract heat time heating time, improved extraction efficiency; The binding silica gel chromatography has improved the quality and the purity of active ingredient, and the method equipment is uncomplicated, and operation is pollution-free easily, for the Yunnan black tea extract preparation provides a kind of improved, respond well method for distilling.Think that through smokeing panel test this product perfuming effect in flue-cured tobacco is obvious: fragrance pass through to send out, plentiful, smoke is pure and mild, fine and smooth, pleasant impression comfort aspect has clear improvement.
The specific embodiment
Through instance method afford of the present invention is further explained below, but do not placed restrictions on the present invention.
Embodiment
The preparation method of Yunnan black tea extract prepares as follows:
Step 1: in the Extraction by Ultrasound jar, add Yunnan black tea tea, add mixed solvent, the water of its ethanol by 2 times of amounts, the propane diols of 2.5 times of amounts, 4.5 times of amounts, the citric acid of 0.05 times of amount are formed.Opening device, temperature remain under 60 ℃, extract 30 minutes, stop operation, and pour out extract after the cooling slightly, filter with 200 mesh filter screens, collect extract.Recrement continues to carry out the second time with said method and extracts, and filters and collects extract for the second time.
Step 2: merge extracted twice liquid, on rotary evaporator, concentrate 65 ℃ of thickening temperatures, vacuum 0.06Mpa;
Step 3: with the proportion that obtains be 1.0 ± 0.02 concentrate with the benzinum of 1 times of amount and the ethyl acetate mixed processing of 5 times of amounts, remove insoluble matter, and reclaim solvent;
Step 4: the concentrate after the step 3 processing is placed on the silica gel column chromatography, as solvent, carry out chromatography, behind the recovery solvent, obtain Yunnan black tea extract with benzinum.
Instance carries out twice, feed intake to be 1000 grams at every turn, for the first time extract 255 grams (recovery rate 25.5%), for the second time extract 245 grams (recovery rate 24.5%), twice average recovery rate is 25.0%;
Detecting its concentrate content is: about 11%, 11 theine of Polyphenols is about 8%, amino acids 0.9%, carbohydrate 2.4%, alkaloid 1.46%.
With the above-mentioned Yunnan black tea extract that makes, press 2/10000ths consumptions of pipe tobacco weight, use 60% dissolve with ethanol, be sprayed onto equably in the pipe tobacco, pipe tobacco is processed cigarette smoke panel test.