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CN106174165A - A kind of short flash extracting method of lycopene - Google Patents

A kind of short flash extracting method of lycopene Download PDF

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Publication number
CN106174165A
CN106174165A CN201610476235.7A CN201610476235A CN106174165A CN 106174165 A CN106174165 A CN 106174165A CN 201610476235 A CN201610476235 A CN 201610476235A CN 106174165 A CN106174165 A CN 106174165A
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lycopene
filtrate
extraction
volume
filtering residue
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唐仕荣
宋慧
李勇
陈尚龙
高兆建
刘恩岐
刘全德
王艳峰
骆乃薇
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Xuzhou University of Technology
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Abstract

本发明公开了一种番茄红素的快速闪式提取方法,其步骤为:先将新鲜番茄通过无水乙醇预处理,再由乙酸乙酯作为溶剂进行闪式提取过程,并通过对比番茄红素标准曲线测算平均提取率。本发明提取时间短、提取效率高,其提取率提取2次每次30s左右的提取率比传统溶剂浸提法提取6h的提取率高80%以上。

The invention discloses a quick flash extraction method of lycopene. The steps are as follows: firstly, fresh tomatoes are pretreated with absolute ethanol, and then ethyl acetate is used as a solvent to carry out the flash extraction process; The standard curve was used to calculate the average extraction rate. The invention has short extraction time and high extraction efficiency, and the extraction rate is 80% higher than that of the traditional solvent extraction method for 6 hours.

Description

一种番茄红素的快速闪式提取方法A kind of rapid flash extraction method of lycopene

技术领域technical field

本发明涉及一种番茄红素的提取方法,尤其涉及一种番茄红素的快速闪式提取方法。The invention relates to a method for extracting lycopene, in particular to a method for extracting lycopene in a flash.

背景技术Background technique

人体番茄红素摄入量的80%以上都是来自番茄,番茄,别名西红柿、洋柿子,属茄科。原产于美洲秘鲁、厄瓜多尔、墨西哥等国家,我国南北广泛栽培。番茄之中含丰富维生素、矿物质、糖类以及钙、钾、铁、锌等多种元素。番茄既能当蔬菜,又可作水果食用。番茄红素是一种不含氧的类胡萝卜素,是一种功能性的自然色素,具有很强的抗氧化性、清除自由基的能力,同时也具有抗衰老的功能,能提高免疫力、预防心脑血管疾病等功效,不仅如此,番茄红素对于防治肿瘤患者、前列腺癌、子宫癌以及免疫低下的中老年人也有良好的功效,是当前食品研究领域的热点。番茄红素世界公认的功能性食品添加剂,具有营养着色双重功效。More than 80% of the human body's lycopene intake comes from tomatoes. Tomatoes, also known as tomatoes and persimmons, belong to the family Solanaceae. Native to America, Peru, Ecuador, Mexico and other countries, it is widely cultivated in the north and south of my country. Tomatoes are rich in vitamins, minerals, sugars, calcium, potassium, iron, zinc and other elements. Tomatoes can be used as both vegetables and fruits. Lycopene is a kind of carotenoid without oxygen. It is a functional natural pigment. It has strong anti-oxidation and the ability to scavenge free radicals. It also has anti-aging functions and can improve immunity. Preventing cardiovascular and cerebrovascular diseases and other effects, not only that, lycopene also has good effects on preventing and treating tumor patients, prostate cancer, uterine cancer, and middle-aged and elderly people with low immunity. It is a hot spot in the field of food research. Lycopene, a world-recognized functional food additive, has dual effects of nutritional coloring.

番茄红素属于脂溶性色素,不溶于水,难溶于强极性溶剂甲醇、乙醇等,可溶于苯、氯仿、乙醚、石油醚、乙烷等有机溶剂,溶于脂肪烃、芳香烃和氯代烃,番茄红素为植物中的天然红色色素,在485nm波长处有一强吸收峰。传统溶剂浸提法使用新鲜番茄提取番茄红素时,新鲜番茄中含有大量的水分,溶剂不容易渗透到细胞内导致提取效率较低,最通常的方式是将番茄干燥、粉碎成粉末后再提取,由于番茄红素为热敏性和光敏性物质,干燥的过程会导致番茄红素含量的损失。Lycopene is a fat-soluble pigment, insoluble in water, hardly soluble in strong polar solvents such as methanol, ethanol, etc., soluble in organic solvents such as benzene, chloroform, ether, petroleum ether, ethane, etc., soluble in aliphatic hydrocarbons, aromatic hydrocarbons and Chlorinated hydrocarbons, lycopene is a natural red pigment in plants, with a strong absorption peak at 485nm wavelength. When the traditional solvent extraction method uses fresh tomatoes to extract lycopene, fresh tomatoes contain a lot of water, and the solvent is not easy to penetrate into the cells, resulting in low extraction efficiency. The most common way is to dry the tomatoes, crush them into powder and then extract them. , Since lycopene is a heat-sensitive and photosensitive substance, the drying process will lead to the loss of lycopene content.

发明内容Contents of the invention

本发明的目的在于提供一种番茄红素的快速闪式提取方法,通过建立乙醇脱水预处理与有机溶剂闪失提取相结合的工艺,控制番茄预处理方式、提取溶剂、提取时间、提取机档位、料液比以提高番茄红素的提取率。The purpose of the present invention is to provide a quick flash extraction method of lycopene, by establishing a process combining ethanol dehydration pretreatment and organic solvent flash extraction, control the tomato pretreatment method, extraction solvent, extraction time, and extraction machine gear , Solid-liquid ratio to increase the extraction rate of lycopene.

为实现上述目的,本发明采用以下技术方案:To achieve the above object, the present invention adopts the following technical solutions:

本发明中一种番茄红素的快速闪式提取方法,具体包括如下具体工艺步骤:A kind of fast flash type extraction method of lycopene among the present invention, specifically comprises following specific process steps:

(1)取样品新鲜番茄洗净切块放入沙冰机,按体积比1:2加入含0.05%BHT的乙醇溶液,搅拌20min,4800r/min离心10min后过滤,滤渣再添加乙醇溶液,再次搅拌20min,4800r/min离心10min后过滤得滤液和滤渣;(1) Take samples of fresh tomatoes, wash and cut them into smoothie machines, add ethanol solution containing 0.05% BHT at a volume ratio of 1:2, stir for 20 minutes, centrifuge at 4800r/min for 10 minutes and filter, then add ethanol solution to the filter residue, and again Stir for 20min, centrifuge at 4800r/min for 10min and filter to obtain filtrate and filter residue;

(2)将步骤(1)得到的番茄滤渣与溶剂按体积比1:35-45放入到闪式提取器中,溶剂为乙酸乙酯或三氯甲烷,调节工作档位至中速(3档)下提取25-35s,离心得到滤液和滤渣;(2) Put the tomato filter residue and solvent obtained in step (1) into the flash extractor at a volume ratio of 1:35-45, the solvent is ethyl acetate or chloroform, and adjust the working gear to medium speed (3 gear) to extract for 25-35s, and centrifuge to obtain filtrate and filter residue;

(3)测定步骤(2)离心后的滤液的体积及其吸光度,测算出滤液中番茄红素的含量及提取率;(3) measure the volume and the absorbance thereof of the centrifuged filtrate of step (2), measure and calculate the content and the extraction rate of lycopene in the filtrate;

(4)取步骤(2)中离心后的番茄滤渣重复步骤(2)的提取过程,离心后得到第二次提取的番茄滤液和滤渣;(4) Get the tomato filter residue after centrifugation in step (2) and repeat the extraction process of step (2), obtain the tomato filtrate and filter residue extracted for the second time after centrifugation;

(5)测定步骤(4)中第二次提取的滤液的体积及其吸光度,测算出滤液中番茄红素的含量及提取率。(5) Measure the volume and absorbance of the filtrate extracted for the second time in step (4), measure and calculate the content and extraction rate of lycopene in the filtrate.

更进一步地,所述步骤(1)中乙醇溶液为无水乙醇溶液。Further, the ethanol solution in the step (1) is absolute ethanol solution.

更进一步地,所述步骤(2)中番茄滤渣与溶剂的体积比为1:40,且所述溶剂为乙酸乙酯。Further, the volume ratio of the tomato filter residue to the solvent in the step (2) is 1:40, and the solvent is ethyl acetate.

更进一步地,所述步骤(3)和步骤(5)中滤液番茄红素含量及提取率的测算方法为:Further, the calculation method of filtrate lycopene content and extraction rate in described step (3) and step (5) is:

A.用苏丹Ⅰ号色素制作番茄红素标准曲线:称取0.0250g苏丹Ⅰ号色素,用无水乙醇移入50mL容量瓶,并定容至刻度,摇匀得番茄红素储备液;准确吸取该储备液10mL于50mL容量瓶,无水乙醇定容至刻度,摇匀;分别吸取0.5、1.0、1.5、2.0、2.5mL于50mL容量瓶,用无水乙醇稀释至刻度,摇匀得浓度分别为0.5、1.0、1.5、2.0、2.5μg/mL的番茄红素标准溶液。以无水乙醇为空白样品,波谱扫描确定最大吸收波长,在该最大吸收波长条件下测定标准溶液吸光度,以浓度为横坐标、吸光度为纵坐标绘制番茄红素标准曲线;A. Prepare lycopene standard curve with Sudan Ⅰ pigment: Weigh 0.0250g of Sudan Ⅰ pigment, transfer it into a 50mL volumetric flask with absolute ethanol, and set the volume to the mark, shake well to obtain lycopene stock solution; accurately draw the Put 10mL of the stock solution in a 50mL volumetric flask, adjust the volume to the mark with absolute ethanol, and shake well; respectively draw 0.5, 1.0, 1.5, 2.0, and 2.5mL into a 50mL volumetric flask, dilute with absolute ethanol to the mark, and shake well to obtain the concentrations of Lycopene standard solutions of 0.5, 1.0, 1.5, 2.0, 2.5 μg/mL. With absolute ethanol as a blank sample, the maximum absorption wavelength is determined by spectral scanning, and the absorbance of the standard solution is measured under the maximum absorption wavelength condition, and the lycopene standard curve is drawn with the concentration as the abscissa and the absorbance as the ordinate;

B.将步骤(2)和(4)中得到离心后的滤液稀释后,根据稀释后滤液番茄红素所测定的吸光度值对照番茄红素标准曲线得出番茄红素的浓度;B. After diluting the centrifuged filtrate obtained in steps (2) and (4), obtain the concentration of lycopene according to the absorbance value measured by the diluted filtrate lycopene against the lycopene standard curve;

C.根据如下公式计算番茄红素提取率:C. Calculate the lycopene extraction rate according to the following formula:

其中,C—根据滤液适当稀释后吸光度换算出来的番茄红素的浓度,μg/mL;Among them, C—the concentration of lycopene converted from the absorbance after appropriate dilution of the filtrate, μg/mL;

V—抽滤得到的滤液体积,mL;V—the volume of filtrate obtained by suction filtration, mL;

m—样品新鲜番茄的质量,g。m—the mass of the sample fresh tomato, g.

本发明的有益效果在于,本发明步骤(1)中采用无水乙醇处理2次有利于水分和醇溶性杂质的脱除而不会造成番茄红素的大量损失,进而有利于提高番茄红素的提取效率和纯度;番茄红素在乙酸乙酯和三氯甲烷中的提取率明显高于其他有机溶剂,且使用乙酸乙酯毒性较小、成本较低;料液比、提取时间和提取档位合理,不会过热造成番茄红素的损失。因此,本发明提取时间短、提取效率高,其提取率提取2次每次30s左右的提取率比传统溶剂浸提法提取6h的提取率高80%以上。The beneficial effects of the present invention are that, in the step (1) of the present invention, the use of absolute ethanol to treat twice is beneficial to the removal of water and alcohol-soluble impurities without causing a large amount of loss of lycopene, which in turn is conducive to improving the concentration of lycopene. Extraction efficiency and purity; the extraction rate of lycopene in ethyl acetate and chloroform is significantly higher than that of other organic solvents, and the use of ethyl acetate has less toxicity and lower cost; solid-liquid ratio, extraction time and extraction gear Reasonable, will not cause loss of lycopene due to overheating. Therefore, the present invention has short extraction time and high extraction efficiency, and its extraction rate is 80% higher than that of the traditional solvent extraction method for 6 hours.

附图说明Description of drawings

图1为本发明所述的一种番茄红素的快速闪式提取方法中的番茄红素标准曲线图。Fig. 1 is a standard curve diagram of lycopene in a quick flash extraction method of lycopene according to the present invention.

具体实施方式detailed description

下面结合附图并通过具体实施方式来进一步说明本发明的技术方案。The technical solutions of the present invention will be further described below in conjunction with the accompanying drawings and through specific implementation methods.

本发明中一种番茄红素的快速闪式提取方法,具体包括如下具体工艺步骤:A kind of fast flash type extraction method of lycopene among the present invention, specifically comprises following specific process steps:

(1)取数十个新鲜番茄洗净切块放入沙冰机,按体积比1:2加入含0.05%BHT的无水乙醇溶液,搅拌20min,4800r/min离心10min后过滤,取得滤渣再添加无水乙醇溶液,再次搅拌20min,4800r/min离心10min后过滤得滤液和滤渣;(1) Take dozens of fresh tomatoes, wash and cut them into smoothie machines, add an absolute ethanol solution containing 0.05% BHT at a volume ratio of 1:2, stir for 20 minutes, centrifuge at 4800r/min for 10 minutes, and filter to obtain the filter residue. Add absolute ethanol solution, stir again for 20min, centrifuge at 4800r/min for 10min and filter to obtain filtrate and filter residue;

(2)取步骤(1)得到的番茄滤渣5克与溶剂按体积比1:40放入到闪式提取器中,溶剂为乙酸乙酯,调节工作档位至3档下提取30s,离心得到番茄滤液和滤渣;(2) Take 5 grams of the tomato filter residue obtained in step (1) and put it into a flash extractor at a volume ratio of 1:40 with a solvent, the solvent is ethyl acetate, adjust the working gear to the third gear and extract for 30 seconds, and centrifuge to obtain Tomato filtrate and residue;

(3)测定步骤(2)离心后的滤液的体积及其吸光度,测算出滤液中番茄红素的含量及提取率:(3) measure the volume and the absorbance thereof of the filtrate after step (2) centrifugation, measure and calculate the content and the extraction rate of lycopene in the filtrate:

(4)取步骤(2)中离心后的番茄滤渣重复步骤(2)的提取过程,二次离心后得到番茄滤液和滤渣;(4) Get the tomato filter residue after centrifugation in step (2) and repeat the extraction process of step (2), obtain tomato filtrate and filter residue after secondary centrifugation;

(5)测定步骤(4)中二次离心后的滤液的体积及其吸光度,测算出滤液中番茄红素的含量及提取率。(5) Measure the volume and absorbance of the filtrate after secondary centrifugation in step (4), measure and calculate the content and extraction rate of lycopene in the filtrate.

在本实例中,步骤(3)和(5)中提取率测算方法具体步骤为:In this instance, the specific steps of the method for calculating the extraction rate in steps (3) and (5) are:

A.用苏丹Ⅰ号色素制作番茄红素标准曲线:称取0.0250g苏丹Ⅰ号色素,用无水乙醇移入50mL容量瓶,并定容至刻度,摇匀得番茄红素储备液;准确吸取该储备液10mL于50mL容量瓶,无水乙醇定容至刻度,摇匀;分别吸取0.5、1.0、1.5、2.0、2.5mL于50mL容量瓶,用无水乙醇稀释至刻度,摇匀得浓度分别为0.5、1.0、1.5、2.0、2.5μg/mL的番茄红素标准溶液。以无水乙醇为空白样品,波谱扫描确定最大吸收波长,在该最大吸收波长条件下测定标准溶液吸光度,以浓度为横坐标、吸光度为纵坐标绘制番茄红素标准曲线;A. Prepare lycopene standard curve with Sudan Ⅰ pigment: Weigh 0.0250g of Sudan Ⅰ pigment, transfer it into a 50mL volumetric flask with absolute ethanol, and set the volume to the mark, shake well to obtain lycopene stock solution; accurately draw the Put 10mL of the stock solution in a 50mL volumetric flask, adjust the volume to the mark with absolute ethanol, and shake well; respectively draw 0.5, 1.0, 1.5, 2.0, and 2.5mL into a 50mL volumetric flask, dilute with absolute ethanol to the mark, and shake well to obtain the concentrations of Lycopene standard solutions of 0.5, 1.0, 1.5, 2.0, 2.5 μg/mL. With absolute ethanol as a blank sample, the maximum absorption wavelength is determined by spectral scanning, and the absorbance of the standard solution is measured under the maximum absorption wavelength condition, and the lycopene standard curve is drawn with the concentration as the abscissa and the absorbance as the ordinate;

B.将步骤(2)和(4)中得到离心后的滤液稀释后,根据稀释后滤液番茄红素所测定的吸光度值对照番茄红素标准曲线得出番茄红素的浓度;B. After diluting the centrifuged filtrate obtained in steps (2) and (4), obtain the concentration of lycopene according to the absorbance value measured by the diluted filtrate lycopene against the lycopene standard curve;

C.根据如下公式计算番茄红素提取率:C. Calculate the lycopene extraction rate according to the following formula:

其中,C—根据滤液适当稀释后吸光度换算出来的番茄红素的浓度,μg/mL;Among them, C—the concentration of lycopene converted from the absorbance after appropriate dilution of the filtrate, μg/mL;

V—抽滤得到的滤液体积,mL;V—the volume of filtrate obtained by suction filtration, mL;

m—样品新鲜番茄的质量,g。m—the mass of the sample fresh tomato, g.

基于上述,测得番茄红素的平均提取率为88.037μg/g,而传统溶剂浸提法提取率一般为47μg/g,可见,本发明中快速闪式提取法兼具快速高效的特点。Based on the above, the measured average extraction rate of lycopene is 88.037 μg/g, while the extraction rate of traditional solvent extraction method is generally 47 μg/g. It can be seen that the flash extraction method in the present invention has the characteristics of fast and high efficiency.

本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。Those skilled in the industry should understand that the present invention is not limited by the above-mentioned embodiments. What are described in the above-mentioned embodiments and the description only illustrate the principle of the present invention. Without departing from the spirit and scope of the present invention, the present invention will also have Variations and improvements are possible, which fall within the scope of the claimed invention. The protection scope of the present invention is defined by the appended claims and their equivalents.

Claims (4)

1. the short flash extracting method of a lycopene, it is characterised in that include following concrete technology step:
(1) taking sample fresh tomato to clean stripping and slicing and put into Ice-making machine, 1:2 adds the ethanol solution containing 0.05%BHT by volume, Stirring 20min, 4800r/min filter after being centrifuged 10min, obtain filtering residue and add ethanol solution again, are again stirring for 20min, 4800r/min filters to get filtrate and filtering residue after being centrifuged 10min;
(2) Fructus Lycopersici esculenti filtering residue step (1) obtained and solvent are during 1:35-45 puts into flash extracter by volume, and solvent is Ethyl acetate or chloroform, extract 25-35s under regulation operation range to middling speed, be centrifuged and obtain filtrate and filtering residue;
(3) determination step (2) is centrifuged volume and the absorbance thereof of rear filtrate, calculates content and the extraction of lycopene in filtrate Rate;
(4) take the Fructus Lycopersici esculenti filtering residue after being centrifuged in step (2) and repeat the extraction process of step (2), after secondary centrifuging, obtain Fructus Lycopersici esculenti filter Liquid and filtering residue;
(5) volume of filtrate after secondary centrifuging and absorbance thereof in determination step (4), calculates containing of lycopene in filtrate Amount and extraction ratio.
The short flash extracting method of a kind of lycopene the most according to claim 1, it is characterised in that described step (1) in, ethanol solution is ethanol solution.
The short flash extracting method of a kind of lycopene the most according to claim 1, it is characterised in that described step (2) in, Fructus Lycopersici esculenti filtering residue is 1:40 with the volume ratio of solvent, and described solvent is ethyl acetate.
The short flash extracting method of a kind of lycopene the most according to claim 1, it is characterised in that described step (3) measuring method of filtrate content of lycopene and extraction ratio is and in (5):
A. lycopene standard curve is made with S Ⅰ pigment: weigh 0.0250g S Ⅰ pigment, move into dehydrated alcohol 50mL volumetric flask, and it is settled to scale, shake up to obtain lycopene storing solution;Accurately draw this storing solution 10mL in 50mL capacity Bottle, dehydrated alcohol is settled to scale, shakes up;Draw 0.5 respectively, 1.0,1.5,2.0,2.5mL is in 50mL volumetric flask, dehydrated alcohol Be diluted to scale, shake up concentration is respectively the lycopene standard solution of 0.5,1.0,1.5,2.0,2.5 μ g/mL.With anhydrous Ethanol is blank sample, and spectral scan determines maximum absorption wavelength, and under the conditions of this maximum absorption wavelength, bioassay standard solution is inhaled Luminosity, with concentration as abscissa, absorbance be vertical coordinate draw lycopene standard curve;
B. after the filtrate dilution after being centrifuged in step (2) and (4), the suction measured according to filtrate lycopene after dilution Shading value comparison lycopene standard curve draws the concentration of lycopene;
C. according to equation below calculating lycopene:
Wherein, C suitably dilute according to filtrate after the absorbance concentration of lycopene that converts out, μ g/mL;
The filtrate volume that V sucking filtration obtains, mL;
The quality of m sample fresh tomato, g.
CN201610476235.7A 2016-06-27 2016-06-27 A kind of short flash extracting method of lycopene Pending CN106174165A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109612957A (en) * 2019-02-22 2019-04-12 济宁医学院 A kind of method of quick detection lycopene

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CN1176577A (en) * 1994-10-31 1998-03-18 马克特辛姆化学工厂有限公司 Stable lycopene concentrate and its preparation method
CN1316468A (en) * 2001-05-15 2001-10-10 北京天纯维通生物技术有限公司 Process for separating and preparing lycopene
CN1328093A (en) * 2001-07-27 2001-12-26 陶法 Process for preparing lycopene
CN1405235A (en) * 2002-10-22 2003-03-26 赵京城 Method for preparing high-purity lycopene

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1176577A (en) * 1994-10-31 1998-03-18 马克特辛姆化学工厂有限公司 Stable lycopene concentrate and its preparation method
CN1316468A (en) * 2001-05-15 2001-10-10 北京天纯维通生物技术有限公司 Process for separating and preparing lycopene
CN1328093A (en) * 2001-07-27 2001-12-26 陶法 Process for preparing lycopene
CN1405235A (en) * 2002-10-22 2003-03-26 赵京城 Method for preparing high-purity lycopene

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109612957A (en) * 2019-02-22 2019-04-12 济宁医学院 A kind of method of quick detection lycopene

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