CN104048933B - In a kind of colorful cotton fibre, flavones content differentiates the method for natural color-cotton - Google Patents
In a kind of colorful cotton fibre, flavones content differentiates the method for natural color-cotton Download PDFInfo
- Publication number
- CN104048933B CN104048933B CN201410263423.2A CN201410263423A CN104048933B CN 104048933 B CN104048933 B CN 104048933B CN 201410263423 A CN201410263423 A CN 201410263423A CN 104048933 B CN104048933 B CN 104048933B
- Authority
- CN
- China
- Prior art keywords
- cotton
- cotton fibre
- colorful
- volume
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Coloring (AREA)
Abstract
The present invention relates to flavones content in a kind of colorful cotton fibre and differentiate the method for natural color-cotton, belong to textile technology field.This discrimination method is: the colorful cotton fibre to be measured after shattering is immersed in 1h in ethanolic solution, adopts ultrasonic assistant to extract and obtains flavone extractive.Flavone extractive is placed in respectively the volumetric flask of 6 25ml by different volumes, in 6 volumetric flasks, adds NaNO respectively
2solution, Al (NO
3)
3solution, NaOH solution carry out chromogenic reaction, are then settled to 25ml with ethanolic solution.The absorbance of the flavone extractive after above-mentioned 6 volumetric flask back warps colour developing constant volume is tested respectively with ultraviolet spectrophotometer.Flavonoids volume concentrations value according to rutin control sample calculate survey flavonoids volume concentrations value in colorful cotton fibre, if flavonoids volume concentrations value is between 0.1411 ~ 0.2314mg/ml in colorful cotton fibre to be measured, then it is dyed cotton; If in colorful cotton fibre to be measured, flavonoids volume concentrations value is 0.7623 ~? between 0.9522mg/ml, then it is natural color-cotton.
Description
Technical field
The present invention relates to flavones content in a kind of colorful cotton fibre and differentiate the method for natural color-cotton, belong to textile technology field.
Background technology
Natural color-cotton refers to that cotton fiber itself has the general designation of the cotton variety of natural colour, existing natural color-cotton utilizes the biotechnologies such as hybridization or gene conduction to cultivate to form, and the generation of its color is caused by the colors deposited gradually in cotton fiber cell Differentiation and development process.At present, the natural color-cotton being successfully applied to textile development only has brown, green two large fundamental types.The features such as natural color-cotton goods have natural in color, soft elegance, quality is soft, goods color is washed darker and darker.This based article, without the need to dyeing, can cut down finished cost, and reduces sewage discharge, is ecological textile worthy of the name, meets people and recover one's original simplicity, and pursues the phychology of pure natural environment protection.
For a long time, the report that most domestic is relevant to natural color-cotton all focuses on the research of form, chromophoric principle, production etc. to natural color-cotton, and few for the investigation and application of natural color-cotton and dyed cotton discrimination method.Natural color-cotton cost ratio common white price of the cotton lattice are high by 50%, and ordinary white cotton is dyed the color close to natural color-cotton by some enterprises, cheats consumers, to fetch high price.In order to China's natural color-cotton industry better develops, urgently an enforceable judging standard and method are formed to the discriminating of natural color-cotton and common dyeing cotton.
At present, go back neither one science, reasonable, quick, succinct discrimination method to the discriminating of natural color-cotton and common dyeing cotton, still rely on experience to carry out coarse differentiation in a lot of situation, reliability is not high.Such as: differentiate from color, natural color-cotton color is not bright-coloured, and dyed cotton color is more bright-coloured.Differentiate from feel, natural color-cotton is soft, and dyed cotton is harder owing to weaving with Final finishing feel.Natural color-cotton adopts cellulase treatment technology, washes softer and softer, and dyed cotton adds softening agent, and water breakthrough just hardens.After natural color-cotton is soaked 6 hours in the washing powder solution of 40 DEG C, use clear water washes clean, observe after dry.Due to natural color-cotton soak for a long time after eliminate the wax coat on cotton fiber surface, therefore color and luster is deepened than before, thus after soaking color burn be genuine piece, otherwise namely belong to pseudo-goods.
In March, 2004, Chinese patent 03141472.9 discloses a kind of preparation method of natural green cotton identification liquid, the formula that this preparation method announces, acid or alkali are added respectively in refining agent 311A, defoamer, bleeding agent KFS, absolute ethyl alcohol, salt and water, mix at the temperature of 15 ~ 40 DEG C.This discrimination method experimental result has deviation, also has no practical application.
In November, 2006, Chinese patent 200610118615.X disclosed a kind of method identifying natural color-cotton.The method by solid state NMR technique qualification natural color-cotton and common dyeing cotton, then is that this method is as secondary evidence by pyrolysis gas chromatography mass spectrometry coupling technique and elemental microanalysis method.But this discrimination method requires high to experimental facilities, be unfavorable for promoting, there are no practical application.
In April, 2007, Chinese patent 200710098853.3 disclosed a kind of discrimination method of natural color-cotton, the method examines under a microscope the Magnifying chromoscopy through the swelling color cotton sample of copper ammon solution, if observe pigment when to be mainly distributed in fiber cell in the shape of a spiral, then this color cotton is natural color-cotton.But this discrimination method subjective factor is large, and when Magnifying chromoscopy shape is not obvious, cannot correctly judge, cannot promote, there are no practical application.
" printing and dyeing " magazine the 6th interim " in color cotton, pigment is on the impact of the microstructure " literary composition that in March, 2004 publishes points out that natural white cotton is identical with the unit cell size of natural color-cotton fiber, but the crystal size of the two is different, from X-ray diffraction measurement result: the crystallinity of white cotton fiber is 80.1%, higher than natural color-cotton (green cotton is 71.5%, and brown cotton is 67.3%).Artificially colored cotton is formed by white cotton dyeing, measured the height of crystallinity, can indirectly differentiate natural color-cotton and dyed cotton by X-diffraction method.But this discrimination method complicated operation, cost is higher, there are no practical application.
" Acta Agronomica Sinica " magazine the 4th phase " research of the natural colorful cotton fibre pigment composition " literary composition published in April, 2005 to extract in cotton fiber flavone compound by methyl alcohol and by drawing the content of flavone compound in Cotton Fiber of Natural Brown Cotton to the ultraviolet spectral analysis of flavone compound extract in 75 DEG C of water-baths.But through many experiments checking, under the condition of the chromogenic reagent usage ratio described in above-mentioned experiment, in cotton fiber, the ultra-violet absorption spectrum of flavone extractive is unstable, cannot judge the concrete content of flavone compound in cotton fiber.
" northwest engineering science and technology institute journal " magazine the 4th phase " extraction of natural color cotton pigment and spectral analysis " one literary grace solvent extraction method that in August, 2007 publishes and nitric acid/ethanol (1:4) oxidizing process extract the pigment of natural colorful cotton fibre.Drawn by the spectral analysis of pigment extract, natural liquor storeroom fiber pigment composition is flavone compound, with adjacent two phenolic hydroxyl groups on B ring.
" inspection and quarantine science " magazine 1-2 phase " research of natural colorful cotton fibre and dyeing processes discrimination method " one literary composition published for 2007 is by testing the ultimate strength of fiber, observe whether fiber profile and square section form and square section COLOR COMPOSITION THROUGH DISTRIBUTION judgement sample are natural color-cotton fiber with microscope projector, but the method DeGrain; Also by comparing natural color-cotton and the colour fastness difference of dyeing processes under Exposure to Sunlight 20h process is differentiated, but the method length consuming time, differentiate the experience of personnel, training degree etc. all can produce considerable influence to result.
" Tianjin textile technology " magazine " discussion of the color cotton fiber qualitative identification method " literary composition published for 2011 is processed green cotton sample under different technology conditions by different reagent, experimental result is compared, analyze, screen, examine under a microscope discovery, the effect of ammoniacal liquor to sample pretreating is the most desirable, the most easily differentiate, it can make the color of green cotton become darker.But this discrimination method is more coarse, inaccurate, there are no practical application.
" textile journal " magazine the tenth phase " the ultrasound-assisted extraction nature forest resource pigment " literary composition published for 2011 is by the ultraviolet spectrum character of ultraviolet spectrophotometry research nature forest resource pigment ethanolic solution, draw the linear relationship of 360nm place light absorption value and pigment concentration, correlativity can reach 0.9992.In cotton fiber, flavone extractive is unstable at the ultraviolet spectrum not carrying out recording under chromogenic reaction, and inaccurate, repeatability is not high.
" Cotton Science " magazine " researchs of the Cotton Fiber of Natural Brown Cotton four kinds of flavonoids HPLC assay methods " literary composition published for 2011 utilizes high-efficient liquid phase chromatogram technology, sets up a kind of method simultaneously detecting four kinds of flavonoid components content such as Cotton Fiber of Natural Brown Cotton cell myricetin, Quercetin, naringenin, Kaempferol.More than these four kinds of the kind of flavonoid substance in cotton fiber, therefore, the method fails to test out the total content of flavones in cotton fiber.
" Wuhan Textile University's journal " magazine the 3rd phase " discriminating of natural color-cotton and dyed cotton " the one literary grace pH value published for 2013 soda acid reversible look change reaction two kinds of methods to natural color-cotton Color influences and cotton fiber pigment extract differentiate natural liquor storeroom and dyeing palm fibre cotton.But this discrimination method mainly relies on artificial judgement, and when color change is not obvious, still cannot accurately judge, the method is more coarse.
" modern textile technology " magazine the 5th phase " pre-test of natural colorful cotton fibre UV-Vis diffuse reflection spectroscopy characteristic " one literary composition published for 2013 is by carrying out spectral analysis to natural color-cotton and dyed cotton, and discovery UV-Vis diffuse reflection spectroscopy effectively can differentiate natural colorful cotton fibre and the basically identical dyed cotton of its color.But this discrimination method requires high to experimental facilities, and need use near-infrared analyzer, Fourier infrared spectrograph, laser Raman spectrometer etc., complicated operation, experimental cost is higher.
Summary of the invention
For above-mentioned existing problems, flavones content in a kind of colorful cotton fibre is the object of the present invention is to provide to differentiate the method for natural color-cotton.
The color of natural color-cotton fiber is caused by the deposition due to coloring matter in fiber finer cell, and the concentration and distribution of coloring matter will directly determine the color trait of fiber.Flavones is the important composition material of natural color-cotton pigment, containing gossypetin, Quercetin, amurensin, 3,4 in natural color-cotton pigment, and the flavonoid substances such as-dihydroxyflavone alcohol.In natural color-cotton, flavones content is more, and pigment content is more, and color is darker.
The color of natural color-cotton be fiber in growth course because pigment deposition is formed, the color of dyed cotton is that white cotton is introduced pigment by colouring method and obtains.Because flavones is expensive, be applied to pharmaceuticals industry more, little for making textile dyestuff.Therefore, the possibility being introduced flavones by colouring method at Bai Mianzhong can be got rid of.Therefore in natural color-cotton and dyed cotton there is gap in flavones content, by experimental results demonstrate, in natural color-cotton, the volumetric concentration value of flavones is between 0.1411 ~ 0.2314mg/ml, in dyed cotton, the volumetric concentration value of flavones is between 0.7623 ~ 0.9522mg/ml, can identify natural color-cotton and dyed cotton according to this.
To achieve these goals, the technical solution used in the present invention is:
In colorful cotton fibre, flavones content differentiates a method for natural color-cotton, and described method is made up of following steps:
1. the extraction of flavones in colorful cotton fibre
By the colorful cotton fibre dry 1h under 60 DEG C of conditions through shattering, under normal temperature, put into 60 ~ 80% ethanolic solutions of 100ml containing 0.5 ~ 1.5gNaOH, bath raio is 1:20 ~ 1:40, under air-proof condition, soak 1h, then adopt ultrasound wave vibration, stir, temperature is 20 ~ 60 DEG C, and the time is 1h, carries out suction filtration 2 times by Suction filtration device to the mixture adding colorful cotton fibre in ethanolic solution, obtain flavone extractive in colorful cotton fibre, for subsequent use;
2. the chromogenic reaction of flavone extractive in colorful cotton fibre
The condition of chromogenic reaction and process are: measure flavone extractive 0.5ml in the colorful cotton fibre extracted by above-mentioned steps successively, 1.0ml, 2.0ml, 4.0ml, 6.0ml, 8.0ml, be positioned in the volumetric flask of 6 25ml respectively, under normal temperature, add the NaNO that concentration is 5% often propping up in volumetric flask
2solution 1.5 ~ 3.5ml, mixing, leaves standstill 5min; Add the Al (NO that concentration is 10% again
3)
3solution 2.5 ~ 4.5ml, mixing, leaves standstill 5min; Add NaOH solution 3 ~ 8ml that concentration is 2mol/L afterwards, mixing, leave standstill 5min, finally add 60 ~ 80% ethanolic solutions and be settled to 25ml, mixing, obtain the solution after the flavone extractive colour developing constant volume of 6 groups of different volumes;
The test of the flavone extractive absorbance after the colour developing constant volume of 3. different volumes
In using ultraviolet spectrophotometer testing procedure 2. respectively 6 groups of different volumes colour developing constant volume after the absorbance of flavone extractive, scanning wave band is 420 ~ 240nm, obtains the absorption values of the flavone extractive after the colour developing constant volume of 6 groups of different volumes;
4. the calculating of flavones relative content in colorful cotton fibre
The absorption values of the flavone extractive after the colour developing constant volume of the 6 groups of different volumes 3. obtained by step, according to unitary linear function, in colorful cotton fibre, the volume-absorbance regression equation of flavones is:
A
1=k
1v
1+ b formula 1
The flavone extractive in rutin is extracted by step method 1., the rutin control sample solution of 6 groups of different volumes is prepared by step method 2., the absorption values of the rutin control sample of 6 groups of different volumes is tested respectively by step method 3., according to unitary linear function, the volume-absorbance regression equation of rutin control sample is:
A
2=k
2v
2+ b formula 2
Wherein A
1for the absorption values of the flavone extractive after colorful cotton fibre colour developing constant volume,
V
1for the volume of flavone extractive in colorful cotton fibre,
K
1for the coefficient of the volume-absorbance regression equation of flavones in colorful cotton fibre,
A
2for the absorption values of rutin control sample solution,
V
2for the volume of rutin control sample solution,
K
2for the coefficient of the volume-absorbance regression equation of rutin control sample,
B is the constant of regression equation;
Work as A
1=A
2, calculate flavonoids volume concentrations value in colorful cotton fibre according to the flavonoids volume concentrations value of rutin control sample;
5. differentiate
4. flavonoids volume concentrations value in colorful cotton fibre is calculated by step, if flavonoids volume concentrations value is between 0.1411 ~ 0.2314mg/ml in colorful cotton fibre, then colorful cotton fibre is dyed cotton, if flavonoids volume concentrations value is between 0.7623 ~ 0.9522mg/ml in colorful cotton fibre, then colorful cotton fibre is natural color-cotton.
Owing to have employed above technical scheme, discrimination method of the present invention, has following characteristics:
One flavones is material impact material and the constituent of pigment thing in natural color-cotton fiber, by extracting flavonoid substance in cotton fiber, instead of the method for extracting directly pigment, the pigment composition difference avoided owing to extracting has an impact to experimental result.
Two in the leaching process of flavones, adopts and add appropriate NaOH in extract, and the techniques such as ultrasound wave vibration, stirring, optimize the extraction process of flavones in colorful cotton fibre further.Adopt extraction process of the present invention, the flavones amount extracted significantly improves, and test result is more stable and accurate.
Three pass through the NaNO adding 5% in the flavone extractive of different volumes
2solution 1.5 ~ 3.5ml, the Al (NO of 10%
3)
3naOH solution 3 ~ the 8ml of solution 2.5 ~ 4.5ml, 2mol/L, obtains the volume-absorbance regression equation A of flavones in natural color-cotton and dyed cotton
1=k
1v
1+ b, according to the volume-absorbance regression equation A of rutin control sample
2=k
2v
2+ b, calculates in natural color-cotton that flavonoids volume concentrations value is between 0.7623 ~ 0.9522mg/ml, and in dyed cotton, flavonoids volume concentrations value is between 0.1411 ~ 0.2314mg/ml.By testing out the flavonoids volume concentrations value in colorful cotton fibre to be identified, can judge that colorful cotton fibre to be identified is dyed cotton or natural color-cotton.
Four the present invention can detect the classification of colorful cotton fibre to be identified fast, and method is simple, and workable, cost is low, and experimental result is stablized.
One times of natural color-cotton price common white price of the cotton lattice, common white cotton is become the color close to natural color-cotton by some enterprises, cheats consumers, to fetch high price.At present enforceable judging standard and method also be there is no to the discriminating of natural color-cotton and dyed cotton.For this problem, the object of the invention is in order to a science, reasonable, quick, succinct discrimination method can be found out.The inventive method is simple, and workable, cost is low, and experimental result is stablized, and is applicable to promoting, will be conducive to China's natural color-cotton industry and better develops.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
In colorful cotton fibre, flavones content differentiates a method for natural color-cotton, and described method is made up of following steps:
1. the extraction of flavones in colorful cotton fibre
The extraction conditions of flavones in cotton fiber is studied, by the colorful cotton fibre dry 1h under 60 DEG C of conditions through shattering, under normal temperature, put into 60 ~ 80% ethanolic solutions of 100ml containing 0.5 ~ 1.5gNaOH, bath raio is 1:20 ~ 1:40, 1h is soaked under air-proof condition, then ultrasound wave vibration is adopted, stir, temperature is 20 ~ 60 DEG C, time is 1h, by Suction filtration device, suction filtration is carried out 2 times to the mixture adding colorful cotton fibre in ethanolic solution, obtain flavone extractive in colorful cotton fibre, for subsequent use, probed into by the major influence factors of orthogonal experiment to the technique extracting flavones in cotton fiber, through great many of experiments, find in extract, add appropriate NaOH, in addition ultrasound wave vibration, the techniques such as stirring, the flavones content extracted significantly improves, test result is more stable and accurate,
2. the chromogenic reaction of flavone extractive in colorful cotton fibre
Color condition is studied, gets flavone extractive in the colorful cotton fibre that certain volume extracts by above-mentioned steps, under normal temperature, add the NaNO that concentration is 5% often propping up in volumetric flask
2solution 1.5 ~ 3.5ml, mixing, leaves standstill 5min; Add the Al (NO that concentration is 10% again
3)
3solution 2.5 ~ 4.5ml, mixing, leaves standstill 5min; Add NaOH solution 3 ~ 8ml that concentration is 2mol/L afterwards, mixing, leave standstill 5min, finally add 60 ~ 80% ethanolic solutions and be settled to 25ml, mixing, obtain the solution after flavone extractive colour developing constant volume.By orthogonal experiment to chromogenic reagent NaNO
2, solution A l (NO
3)
3the concentration of solution, NaOH solution and consumption have carried out probing in a large number.By the abosrption spectrogram of solution after ultraviolet spectrophotometer test colour developing, draw best color condition.
The condition of chromogenic reaction and process are: on the basis of known optimum extraction condition and best color condition, arrange the gradient group of different volumes.Measure the extract 0.5ml of flavones in the colorful cotton fibre extracted by above-mentioned steps successively, 1.0ml, 2.0ml, 4.0ml, 6.0ml, 8.0ml, be positioned in 6 25ml volumetric flasks respectively, under normal temperature, add the NaNO that concentration is 5% often propping up in volumetric flask
2solution 1.5 ~ 3.5ml, mixing, leaves standstill 5min; Add the Al (NO that concentration is 10% again
3)
3solution 2.5 ~ 4.5ml, mixing, leaves standstill 5min; Add NaOH solution 3 ~ 8ml that concentration is 2mol/L afterwards, mixing, leave standstill 5min, finally add 60 ~ 80% ethanolic solutions and be settled to 25ml, mixing, obtain the solution after the flavone extractive colour developing constant volume of 6 groups of different volumes.
The test of the flavone extractive absorbance after the colour developing constant volume of 3. different volumes
In using ultraviolet spectrophotometer testing procedure 2. respectively 6 groups of different volumes colour developing constant volume after the absorbance of flavone extractive, scanning wave band is 420 ~ 240nm, obtains the absorption values of the flavone extractive after the colour developing constant volume of 6 groups of different volumes;
4. the calculating of flavones relative content in colorful cotton fibre
The absorption values of the flavone extractive after the colour developing constant volume of the 6 groups of different volumes 3. obtained by step, according to unitary linear function, in colorful cotton fibre, the volume-absorbance regression equation of flavones is:
A
1=k
1v
1+ b formula 1
The flavone extractive in rutin is extracted by step method 1., the rutin control sample solution of 6 groups of different volumes is prepared by step method 2., the absorption values of the rutin control sample of 6 groups of different volumes is tested respectively by step method 3., according to unitary linear function, the volume-absorbance regression equation of rutin control sample is:
A
2=k
2v
2+ b formula 2
Wherein A
1for the absorption values of the flavone extractive after colorful cotton fibre colour developing constant volume,
V
1for the volume of flavone extractive in colorful cotton fibre,
K
1for the coefficient of the volume-absorbance regression equation of flavones in colorful cotton fibre,
A
2for the absorption values of rutin control sample solution,
V
2for the volume of rutin control sample solution,
K
2for the coefficient of the volume-absorbance regression equation of rutin control sample,
B is the constant of regression equation;
Pass in colorful cotton fibre between flavones content and flavonoids volume concentrations and volume is:
M
1=C
1× V
1formula 3
Pass in rutin control sample between flavones content and flavonoids volume concentrations and volume is:
M
2=C
2× V
2formula 4
Wherein m
1for in colorful cotton fibre when flavone extractive volume is V
1time flavones content,
C
1for flavonoids volume concentrations in colorful cotton fibre,
M
2for in rutin control sample when flavone extractive volume is V
2time flavones content,
C
2for flavonoids volume concentrations in rutin control sample.
When the flavones content in colorful cotton fibre is identical with the flavones content in rutin control sample, the absorbance recorded after the same terms colour developing is identical, namely works as m
1=m
2time, A
1=A
2.
Work as m
1=m
2time, by formula 3, formula 4 can obtain
Work as A
1=A
2time, by formula 1, formula 2 can obtain
Can be obtained by formula 5,6
Namely
Formula 8
Work as A
1=A
2, calculate flavonoids volume concentrations value in colorful cotton fibre according to the flavonoids volume concentrations value of rutin control sample;
5. differentiate
4. flavonoids volume concentrations value in colorful cotton fibre is calculated by step, if flavonoids volume concentrations value is between 0.1411 ~ 0.2314mg/ml in colorful cotton fibre, then colorful cotton fibre is dyed cotton, if flavonoids volume concentrations value is between 0.7623 ~ 0.9522mg/ml in colorful cotton fibre, then colorful cotton fibre is natural color-cotton.
Specific embodiment
Embodiment 1
By the Cotton Fiber of Natural Brown Cotton to be identified dry 1h under 60 DEG C of conditions through shattering, take wherein 5.0g, put into 70% ethanolic solution of 100ml containing 0.5gNaOH, bath raio is 1:20, adds a cover and soaks 1h, and adopt ultrasound wave vibration, stir, temperature 50 C, the time is 1h.Suction filtration is carried out 2 times, flavone extractive in obtained Cotton Fiber of Natural Brown Cotton by Suction filtration device.Measure flavone extractive 0.5ml in the Cotton Fiber of Natural Brown Cotton obtained by above-mentioned steps successively, 1.0ml, 2.0ml, 4.0ml, 6.0ml, 8.0ml, be positioned in 6 25ml volumetric flasks, in volumetric flask, first add the NaNO that concentration is 5%
2solution 2.5ml, mixing, leaves standstill 5min; Add the Al (NO that concentration is 10% again
3)
3solution 3.5ml, mixing, leaves standstill 5min; Add the NaOH solution 5ml that concentration is 2mol/L afterwards, mixing, leave standstill 5min, finally add 70% ethanolic solution and be settled to 25ml, mixing, sealing is added a cover.Solution ultraviolet spectrophotometer after colour developing is tested its absorbance respectively, and wherein, scanning wave band is 420 ~ 240nm.Volume-absorbance the regression equation of flavones in obtained Cotton Fiber of Natural Brown Cotton, according to the volume-absorbance regression equation of rutin control sample, calculating flavonoids volume concentrations value in Cotton Fiber of Natural Brown Cotton to be identified is 0.9272mg/ml.Identification result: this Cotton Fiber of Natural Brown Cotton to be identified is natural color-cotton.
Embodiment 2
By the Cotton Fiber of Natural Brown Cotton to be identified dry 1h under 60 DEG C of conditions through shattering, taking wherein 3.33g, putting into 60% ethanolic solution of 100ml containing 1.0gNaOH; bath raio is 1:30, adding a cover and soak 1h, adopt ultrasound wave vibration, stir; temperature 40 DEG C, the time is 1h.Suction filtration is carried out 2 times, flavone extractive in obtained Cotton Fiber of Natural Brown Cotton by Suction filtration device.Measure flavone extractive 0.5ml in the Cotton Fiber of Natural Brown Cotton obtained by above-mentioned steps successively, 1.0ml, 2.0ml, 4.0ml, 6.0ml, 8.0ml, be positioned in 6 25ml volumetric flasks, in volumetric flask, first add the NaNO that concentration is 5%
2solution 2.5ml, mixing, leaves standstill 5min; Add the Al (NO that concentration is 10% again
3)
3solution 3.5ml, mixing, leaves standstill 5min; Add the NaOH solution 3ml that concentration is 2mol/L afterwards, mixing, leave standstill 5min, finally add 60% ethanolic solution and be settled to 25ml, mixing, sealing is added a cover.Solution ultraviolet spectrophotometer after colour developing is tested absorbance, and wherein, scanning wave band is 420 ~ 240nm.Volume-absorbance the regression equation of flavones in obtained Cotton Fiber of Natural Brown Cotton, according to the volume-absorbance regression equation of rutin control sample, calculating flavonoids volume concentrations value in Cotton Fiber of Natural Brown Cotton to be identified is 0.1421mg/ml.Identification result: this Cotton Fiber of Natural Brown Cotton to be identified is dyed cotton.
Embodiment 3
By the Cotton Fiber of Natural Brown Cotton to be identified dry 1h under 60 DEG C of conditions through shattering, take wherein 2.5g, put into 80% ethanolic solution of 100ml containing 1.5gNaOH, bath raio is 1:40, adds a cover and soaks 1h, and adopt ultrasound wave vibration, stir, temperature 60 C, the time is 1h.Suction filtration is carried out 2 times, flavone extractive in obtained Cotton Fiber of Natural Brown Cotton by Suction filtration device.Measure flavone extractive 0.5ml in the Cotton Fiber of Natural Brown Cotton obtained by above-mentioned steps successively, 1.0ml, 2.0ml, 4.0ml, 6.0ml, 8.0ml, be positioned in 6 25ml volumetric flasks, in volumetric flask, first add the NaNO that concentration is 5%
2solution 3.5ml, mixing, leaves standstill 5min; Add the Al (NO that concentration is 10% again
3)
3solution 4.5ml, mixing, leaves standstill 5min; Add the NaOH solution 8ml that concentration is 2mol/L afterwards, mixing, leave standstill 5min, finally add 80% ethanolic solution and be settled to 25ml, mixing, sealing is added a cover.Solution ultraviolet spectrophotometer after colour developing is tested absorbance, and wherein, scanning wave band is 420 ~ 240nm.Volume-absorbance the regression equation of flavones in obtained Cotton Fiber of Natural Brown Cotton, according to the volume-absorbance regression equation of rutin control sample, calculating flavonoids volume concentrations value in Cotton Fiber of Natural Brown Cotton to be identified is 0.2019mg/ml.Identification result: this Cotton Fiber of Natural Brown Cotton to be identified is dyed cotton.
Claims (1)
1. in colorful cotton fibre, flavones content differentiates a method for natural color-cotton, it is characterized in that: described method is made up of following steps:
1. the extraction of flavones in colorful cotton fibre
By the colorful cotton fibre dry 1h under 60 DEG C of conditions through shattering, under normal temperature, put into 60 ~ 80% ethanolic solutions of 100ml containing 0.5 ~ 1.5gNaOH, bath raio is 1:20 ~ 1:40, under air-proof condition, soak 1h, then adopt ultrasound wave vibration, stir, temperature is 20 ~ 60 DEG C, and the time is 1h, carries out suction filtration 2 times by Suction filtration device to the mixture adding colorful cotton fibre in ethanolic solution, obtain flavone extractive in colorful cotton fibre, for subsequent use;
2. the chromogenic reaction of flavone extractive in colorful cotton fibre
The condition of chromogenic reaction and process are: measure flavone extractive 0.5ml in the colorful cotton fibre extracted by above-mentioned steps successively, 1.0ml, 2.0ml, 4.0ml, 6.0ml, 8.0ml, be positioned in the volumetric flask of 6 25ml respectively, under normal temperature, add the NaNO that concentration is 5% often propping up in volumetric flask
2solution 1.5 ~ 3.5ml, mixing, leaves standstill 5min; Add the Al (NO that concentration is 10% again
3)
3solution 2.5 ~ 4.5ml, mixing, leaves standstill 5min; Add NaOH solution 3 ~ 8ml that concentration is 2mol/L afterwards, mixing, leave standstill 5min, finally add 60 ~ 80% ethanolic solutions and be settled to 25ml, mixing, obtain the solution after the flavone extractive colour developing constant volume of 6 groups of different volumes;
The test of the flavone extractive absorbance after the colour developing constant volume of 3. different volumes
In using ultraviolet spectrophotometer testing procedure 2. respectively 6 groups of different volumes colour developing constant volume after the absorbance of flavone extractive, scanning wave band is 420 ~ 240nm, obtains the absorption values of the flavone extractive after the colour developing constant volume of 6 groups of different volumes;
4. the calculating of flavones relative content in colorful cotton fibre
The absorption values of the flavone extractive after the colour developing constant volume of the 6 groups of different volumes 3. obtained by step, according to unitary linear function, in colorful cotton fibre, the volume-absorbance regression equation of flavones is:
A
1=k
1v
1+ b formula 1
The flavone extractive in rutin is extracted by step method 1., the rutin control sample solution of 6 groups of different volumes is prepared by step method 2., the absorption values of the rutin control sample of 6 groups of different volumes is tested respectively by step method 3., according to unitary linear function, the volume-absorbance regression equation of rutin control sample is:
A
2=k
2v
2+ b formula 2
Wherein A
1for the absorption values of the flavone extractive after colorful cotton fibre colour developing constant volume,
V
1for the volume of flavone extractive in colorful cotton fibre,
K
1for the coefficient of the volume-absorbance regression equation of flavones in colorful cotton fibre,
A
2for the absorption values of rutin control sample solution,
V
2for the volume of rutin control sample solution,
K
2for the coefficient of the volume-absorbance regression equation of rutin control sample,
B is the constant of regression equation;
Work as A
1=A
2time, calculate flavonoids volume concentrations value in colorful cotton fibre according to the flavonoids volume concentrations value of rutin control sample;
5. differentiate
4. flavonoids volume concentrations value in colorful cotton fibre is calculated by step, if flavonoids volume concentrations value is between 0.1411 ~ 0.2314mg/ml in colorful cotton fibre, then colorful cotton fibre is dyed cotton, if flavonoids volume concentrations value is between 0.7623 ~ 0.9522mg/ml in colorful cotton fibre, then colorful cotton fibre is natural color-cotton.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410263423.2A CN104048933B (en) | 2014-06-13 | 2014-06-13 | In a kind of colorful cotton fibre, flavones content differentiates the method for natural color-cotton |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410263423.2A CN104048933B (en) | 2014-06-13 | 2014-06-13 | In a kind of colorful cotton fibre, flavones content differentiates the method for natural color-cotton |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104048933A CN104048933A (en) | 2014-09-17 |
| CN104048933B true CN104048933B (en) | 2016-03-30 |
Family
ID=51502053
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410263423.2A Expired - Fee Related CN104048933B (en) | 2014-06-13 | 2014-06-13 | In a kind of colorful cotton fibre, flavones content differentiates the method for natural color-cotton |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104048933B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106568767B (en) * | 2016-10-25 | 2018-07-20 | 浙江理工大学 | Quickly differentiate the method for true and false natural color cotton and its product |
| CN106645251B (en) * | 2016-12-19 | 2019-05-03 | 宁波出入境检验检疫局检验检疫技术中心 | A kind of method of quick identification natural color cotton |
| CN107271435B (en) * | 2017-05-31 | 2019-11-12 | 湖北省纤维检验局 | A kind of qualitative identification method of natural color cotton product |
| CN111505004B (en) * | 2020-04-21 | 2021-04-06 | 东华大学 | Method for identifying natural colored cotton and dyed cotton |
| CN116350565B (en) * | 2023-06-01 | 2023-12-15 | 广州巴宝莉化妆品有限公司 | Method for purifying active substance stock solution of fresh flowers |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1959389A (en) * | 2006-11-22 | 2007-05-09 | 东华大学 | Method for identifying natural color cotton |
| CN101046057B (en) * | 2007-04-28 | 2010-05-26 | 北京服装学院 | Method of discriminating natural color cotton |
-
2014
- 2014-06-13 CN CN201410263423.2A patent/CN104048933B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN104048933A (en) | 2014-09-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104048933B (en) | In a kind of colorful cotton fibre, flavones content differentiates the method for natural color-cotton | |
| Colombini et al. | Colour fading in textiles: A model study on the decomposition of natural dyes | |
| Cesaratto et al. | Recent advances on the analysis of polychrome works of art: SERS of synthetic colorants and their mixtures with natural dyes | |
| CN107121514B (en) | Method that is a kind of while detecting 24 kinds of synthetic food colors in cigarette packaging material | |
| CN103235059A (en) | Establishment method and application of mass spectrum database of prohibited colorant in foods | |
| CN102175648A (en) | Method for distinguishing variety of fritillaria and detecting total alkaloid content of fritillaria by virtue of near infrared spectrum | |
| CN108414675B (en) | Method for rapidly determining low-concentration boric acid in aqueous solution by using pH meter | |
| CN104897665A (en) | One-step color-development screening method for banned azo-dye in dyeing textiles | |
| CN101718684B (en) | On-line soft-measuring method and system for fabric color during batch dyeing | |
| CN108760712B (en) | Cultural relic light damage determination method based on Raman spectrum analysis | |
| CN105548055A (en) | Determination method of soluble sugar in cotton fiber | |
| CN108827907A (en) | It is a kind of based near infrared spectrum to the rapid assay methods of color cotton coloration | |
| CN104655580A (en) | Method for quickly determining content of alpha-cellulose in dissolving pulp | |
| CN106568767B (en) | Quickly differentiate the method for true and false natural color cotton and its product | |
| CN103076291B (en) | A kind of tricolor dye and the method for detecting linen-cotton two kinds of fiber blend ratios | |
| US9958370B2 (en) | Method for measuring diffusion performance of acid dye in color paste | |
| CN101187635A (en) | Method for identifying textile fibers based on Raman spectra qualitative identification | |
| CN103389318B (en) | A kind of method differentiating true and false beef and mutton | |
| CN104614319A (en) | A method of digitized analysis of compatibility of a dye composition by adoption of a spectrometer | |
| CN104634632A (en) | Method for stripping dyes on dyed silk fabrics | |
| CN100494995C (en) | Leather Cr6+ automatic analysis method | |
| Suva | Opuntia ficus indica (L.) fruit extract as natural indicator in acid-base titration | |
| CN106198811A (en) | Quickly measure water and aquatic products Malachite Green and the test kit of crystal violet and method | |
| CN110389166A (en) | The rapid detection method of heavy metal limit in a kind of food additives | |
| CN101804082B (en) | Method for identifying cordyceps sinensis powder through microscopic dyeing |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160330 Termination date: 20190613 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |