CN107607668A - A kind of method of glycerine in dual wavelength thin-layer chromatography scanning quantitation analysis krill glycerine crude extract - Google Patents
A kind of method of glycerine in dual wavelength thin-layer chromatography scanning quantitation analysis krill glycerine crude extract Download PDFInfo
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- CN107607668A CN107607668A CN201710729980.2A CN201710729980A CN107607668A CN 107607668 A CN107607668 A CN 107607668A CN 201710729980 A CN201710729980 A CN 201710729980A CN 107607668 A CN107607668 A CN 107607668A
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Abstract
The invention discloses a kind of method that dual wavelength thin-layer chromatography scanning quantitation analyzes glycerine in krill glycerine crude extract, this method directly can carry out analysis detection to krill glycerine crude extract, easy to operate, quick, and result of the test is accurate, reliable.Specifically, this method includes:1) glycerine standard items are dissolved in methanol, standard items liquid is made;2) using glycerine crude extract as sample liquid and standard items liquid spotting in same thin layer silica gel H plate, with dichloromethane:Methanol=5:1 is solvent, the 30min of pre-equilibration 20, thin-layer developing;3) after expansion terminates, thin layer silica gel plate is taken, is dried, dyed;4) thin-layer chromatogram scanner carries out double-wavelength scan, and by examination criteria product liquid and the scanning integrating peak areas value of sample liquid, glycerol content in krill glycerine crude extract is calculated.
Description
Technical field
The invention belongs to food and chemical analysis technical field, and in particular to a kind of dual wavelength thin-layer chromatography scanning quantitation point
The method for analysing glycerine in krill glycerine crude extract.
Background technology
Glycerine, also known as Glycerin, glycerine;Molecular formula is C3H8O3, molecular weight 92.09,290.9 DEG C of boiling point, it is
A kind of thick liquid of no color or smell, it is pleasantly sweet, it is soluble in alcohol and water.Because glycerine has good solvability and nontoxic
Property, it is usually used in food the solvent as many flavorants and food coloring, meanwhile, glycerine can play moist work to skin
With being widely used in cosmetics.The glycerine of pharmaceutical grades, can be used as in medicine lubricant, sweetener, bleeding agent and
Antifreeze.Glycerine usually coordinates as antifreeze with water to be used, and 66.7% glycerine water solution freezing point is minimum, is -46.5 DEG C.It is sweet
Oil is found in a variety of cold-resistant animal bodies, is a kind of important small molecule antifreeze.Due to having many uses for glycerine, therefore,
Its content is detected to have great importance.
Krill, it is a kind of crustacean in the Antarctic Continent waters for living in Antarctic Ocean, is the pass of Antarctic ecosystems
Key species.Krill reserves are huge, about share 500,000,000 tons, and are lived more in a manner of gregarious, easily collection fishing.Krill
Live in throughout the year under Antarctic Ice, can endure cold environment, the presence of glycerine in krill, pole cold air may be adapted to it and is waited
It is relevant, be advantageous to existence and the physiological activity of krill.
The assay method of glycerol content is more both at home and abroad at present, mainly there is periodate oxidation method, cu2+ Chelatocolorimetries, sweet
It is oily kinase method, ultraviolet -- visible spectrophotometry, high performance liquid chromatography, gas chromatography, near infrared spectroscopy and atom
Absorption process etc..Periodate oxidation method is easy to operate, but is influenceed (such as pH) by factors, and condition is difficult to control, and need through
Cross more complicated purification step.Colorimetric method and UV-VIS spectrophotometry result precision are high, and error is small, but needs to exclude
The interference of color, and content astaxanthin is high in krill, in bright-coloured red, has extreme influence for detection, and remove
The step of astaxanthin, is cumbersome, complicated.High performance liquid chromatography and gas chromatography detection accuracy are high, are not easy by other materials
Interference, but be the blocking for avoiding instrument before detecting, also need to carry out multiple impurity elimination steps, and instrument is costly, detection time length.
And glycerine need to be purified out by infrared chromatography, complex operation.
The content of the invention
For above-mentioned the deficiencies in the prior art, inventor is through long-term technology and practical exploration, there is provided a kind of dual wavelength is thin
The method for analysing glycerine in scanning quantitation analysis krill glycerine crude extract layer by layer, this method can be directly thick to krill glycerine
Extract carries out analysis detection, easy to operate, quick, and result of the test is accurate, reliable.
Specifically, the present invention relates to following technical scheme:
The first aspect of the invention, there is provided a kind of dual wavelength thin-layer chromatography scanning quantitation analysis krill glycerine is thick
The method of glycerine, specific steps include in extract:
1) glycerine standard items are dissolved in methanol, standard items liquid is made;
2) using glycerine crude extract as sample liquid and standard items liquid spotting in same thin layer silica gel H plate, with dichloromethane:
Methanol=5:1 is solvent, pre-equilibration 20-30min, thin-layer developing;
3) after expansion terminates, thin layer silica gel plate is taken, is dried, dyed;
4) thin-layer chromatogram scanner carries out double-wavelength scan, passes through examination criteria product liquid and the scanning integrating peak areas of sample liquid
Value, is calculated glycerol content in krill glycerine crude extract;
Wherein, in step 1), the concentration of the standard items liquid is 1mg/ml;
In step 2), thin-layer developing exhibition is away from for 8~10cm (be preferably 9cm);
In step 3), with the spray plate dyeing of alkalinity potassium permanganate developer, then toasted 2~3 minutes at 60~70 DEG C,
Under purple background, glycerine displaing yellow;
In step 4), dual wavelength parameter is specially Detection wavelength 276nm, reference wavelength 550nm;
With the quality (μ g) of glycerine standard items for abscissa (X), integrating peak areas value (AU) is ordinate (Y), is returned
It is Y=-7025.028+6167.319 × X, r=0.99928, sdv=2.10% to return equation;With above-mentioned regression equation to sample
Glycerine carries out analysis detection in liquid;
Wherein, the preparation method of the krill glycerine crude extract is:
Fresh krill and absolute ethyl alcohol are pressed into mass volume ratio 1g:(10-15) ml is mixed, ultrasonic extraction, filtrate
It is evaporated, dissolves to obtain glycerine crude extract with absolute ethyl alcohol.
The condition of the ultrasonic extraction is:30~40 DEG C, 250~350W, 30~50kHz, extraction time be 0.8~
1.5h;
Preferably, the condition of the ultrasonic extraction is:35 DEG C, 300W, 40kHz, extraction time 1h, in triplicate, receive
Collect filtrate;
It should be noted that although it is a kind of conventional analysis to carry out quantitative analysis detection using Tlc-dm Method
Method, still, glycerine of the invention are extracted from krill and obtained, and the raw material used when being detected is glycerine
Crude extract, also contain lipid material, volatile oil and other compositions in the crude extract, due to krill complicated component, therefore
When carrying out quantitative detection using Tlc-dm Method to glycerine crude extract, other interference components for how avoiding introducing are to inspection
The influence of result is surveyed, turns into the important content of the application research.
In thin layer scanning detection, the selection of solvent and developer is very crucial factor, as previously described, because southern
Complicated component in the krill of pole, the application are directly detected from glycerine crude extract, interference component are inevitably introduced, thin
During layer expansion, solvent and its ratio selection are improper, on the one hand can influence the formation of glycerine sampling point, cause hangover etc. existing
As;On the other hand disturbed specimen point can be also formed in thin layer panel, so as to directly affect testing result so that testing result is not
Accurately, premenstruum (premenstrua) experiment is found, due in glycerine crude extract, existing highly polar composition, also having low pole composition, species is very
It is numerous and diverse, therefore the present invention has attempted a variety of solvents and combination during the selection of solvent, and constantly adjust ratio ginseng
Number, but result is unsatisfactory, solvent separating effect is poor, there is interference spot at the upper-lower position of measure spot
Occur, cause that gained measurement result is higher, and inventor has found in continuous explorative experiment, make to deploy using dichloromethane and methanol
Agent and the two volume ratio be 5:In the case of 1, the glycerine in glycerine crude extract has obtained good separation, and RfValue is suitable
Close, be very beneficial for quantitative determining, and once deviate the volume ratio, then expansion separation is deteriorated, the separating effect not reached.Together
When, glycerine crude extract is dissolved using ethanol not only reduces the tedious steps that lysate is changed in chromatography process, avoids loss of product,
Improve the degree of accuracy;Inventors be surprised to learn that under this thin-layer chromatography system, using its expansion point of the crude extract of absolute ethyl alcohol dissolving
From significant effect better than methanol, dichloromethane other solvents.
Developer species is various, and because the application is to use dual-wavelength lamellar scanning to carry out quantitative analysis, therefore it is aobvious
Chromatic sensitivity is very big for final result influence, and developer and solvent are closely related, in addition composition in glycerine crude extract
Complexity, different solvents coordinate with developer, and caused result is entirely different, and final inventor determines to adopt in thin-layer chromatography
By the use of alkalinity potassium permanganate as developer, after violet exposure, yellow spotting is clear, high sensitivity, and glycerine shows spot
Adjacent locations are noiseless spot, it is easy to subsequently use the scanning of double wave long wave layer to carry out quantitative analysis, meanwhile, inventor has found, such as
The glycerine crude extract is carried out further chromatographic purifying by fruit, using thin-layer chromatography system of the present invention, then the huge drop of sensitivity, and spot mould
Paste, can not carry out quantitative assessment at all.
Meanwhile the selection of scanning wavelength is equally important to the application quantitative analysis, inventor is carrying out wavelength selection
During, found through experiment, between wavelength 200-300nm, scanning effect is preferable, final to determine by continually scanning for detecting
276nm wavelength is selected as Detection wavelength, and selects to be used as reference wavelength at the minimum 550nm of glycerine absorbance, so as to maximum
Degree excludes background, dyeing and the interference at peak, improves the sensitivity and the degree of accuracy of detection.
The invention also discloses application of the above-mentioned detection method in glycerine in quantitative determining krill glycerine crude extract.
Beneficial effects of the present invention:
The present invention establishes the dual-wavelength lamellar scanning quantitative analysis of the glycerine crude extract to being extracted from krill first
Method, detection method is simple, accurate, reliable, and stability is high;Because the present invention is that directly the glycerine of EtOH Sonicate extraction is slightly carried
Carry out direct quantitative is taken, it is easy to operate without the purge process by complexity, it is only necessary to and with simple instrument, reagent is few,
Detection is rapid, and effect is good;
Meanwhile by analyzing thin layer scanning the optimum choice of parameter and reagent in each step process so that the present invention
Detection method accuracy, repeatability, the rate of recovery are significantly improved, so as to really realize to single component in complex extraction thing
Quick and precisely property detection.
Brief description of the drawings
Fig. 1 is the thin-layer developing figure of sample liquid and titer in embodiment 1, wherein, 1 is glycerine crude extract, and 2 be glycerine mark
Quasi- product, point A are the glycerine in crude extract, and point B is glycerine in standard items;
Fig. 2 is that the sample liquid of embodiment 1 and standard items liquid all-wave length overlap scanning curve, and wherein curve 1 is sample liquid all-wave
Long scan curve, curve 2 are standard items liquid full wavelength scanner curve.
Embodiment
It is noted that described further below is all exemplary, it is intended to provides further instruction to the application.It is unless another
Indicate, all technologies used herein and scientific terminology are with usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in this manual using term "comprising" and/or " bag
Include " when, it indicates existing characteristics, step, operation, device, component and/or combinations thereof.
As background technology is introduced, although the assay method of existing glycerol content is more, detection method be present
Complex steps, the sensitive low defect of detection;
In view of this, in a kind of embodiment of the invention, there is provided a kind of dual wavelength thin-layer chromatography scanning quantitation point
The method for analysing glycerine in krill glycerine crude extract, step include:
1) glycerine standard items are dissolved in methanol, standard items liquid is made;
2) using glycerine crude extract as sample liquid and standard items liquid spotting in same thin layer silica gel H plate, with dichloromethane:
Methanol=5:1 is solvent, pre-equilibration 20-30min, thin-layer developing;
3) after expansion terminates, thin layer silica gel plate is taken, is dried, dyed;
4) thin-layer chromatogram scanner carries out double-wavelength scan, passes through examination criteria product liquid and the scanning integrating peak areas of sample liquid
Value, is calculated glycerol content in krill glycerine crude extract;
Wherein, in step 1), the concentration of the standard items liquid is 1mg/ml;
In step 2), thin-layer developing exhibition is away from for 8~10cm (be preferably 9cm);
In step 3), with the spray plate dyeing of alkalinity potassium permanganate developer, then toasted 2~3 minutes at 60~70 DEG C,
Under purple background, glycerine displaing yellow;
Wherein, alkalinity potassium permanganate developer is configured to be divided into:1.5g KMnO4, 10g K2CO3, 1.25mL 10%
NaOH, 200mL tri-distilled water;
In step 4), dual wavelength parameter is specially Detection wavelength 276nm, reference wavelength 550nm;
With the quality (μ g) of glycerine standard items for abscissa (X), integrating peak areas value (AU) is ordinate (Y), is returned
It is Y=-7025.028+6167.319 × X, r=0.99928, sdv=2.10% to return equation;With above-mentioned regression equation to sample
Glycerine carries out analysis detection in liquid;
In the still another embodiment of the present invention, there is provided the preparation method of the krill glycerine crude extract, tool
Body is:
Fresh krill and absolute ethyl alcohol are pressed into mass volume ratio 1g:(10-15) ml is mixed, ultrasonic extraction, filtrate
It is evaporated, dissolves to obtain glycerine crude extract with absolute ethyl alcohol.
The condition of the ultrasonic extraction is:30~40 DEG C, 250~350W, 30~50kHz, extraction time be 0.8~
1.5h;
In the still another embodiment of the present invention, the condition of the ultrasonic extraction is:35 DEG C, 300W, 40kHz, extraction
Time is 1h, in triplicate, collects filtrate;
Explanation is further explained to the present invention by the following examples, but is not construed as limiting the invention.
Embodiment 1
The krill 40g of freeze-drying is taken, is crushed with high-speed tissue mashing machine, adds absolute ethyl alcohol 600mL,
35 DEG C, ultrasonic extraction in 300w, 40kHz supersonic wave cleaning machine, extract 1h, filter extract solution, collect filtrate.In triplicate,
Merge all filtrates.Filtrate is evaporated to dryness in Rotary Evaporators, revolving temperature is 35 DEG C, and revolving residue is dissolved in
In 10ml absolute ethyl alcohols, the crude extract of glycerine is obtained.
Precision weighs 1.000mg glycerine standard items and is dissolved in 1.0mL methanol, obtains the glycerine standard items that concentration is 1mg/mL
Solution.
By sample liquid and standard items liquid point in (5 × 10cm on same High Performance Thin silica gel H plate2) on, solvent volume
Than for dichloromethane:Methanol=5:1, solvent is added into expansion cylinder (10 × 12 × 15cm3), pre-equilibration 30min at room temperature,
High Performance Thin plate is placed into, when exhibition is away from 9cm is reached, expansion terminates, and is dried after plate is deployed.Dyed, used with alkalinity potassium permanganate
Hair-dryer heating 3min (60 DEG C), under purple background, glycerine displaing yellow.Dual wavelength is carried out with CAMAG thin-layer chromatogram scanners-III
Scanning, Detection wavelength 276nm, reference wavelength 550nm, passes through standard items and the scanning peak area quantification of sample.Obtain drying south
The content of glycerine is 1.12mg/g in the krill of pole.
Embodiment 2
The krill 40g of freeze-drying is taken, is crushed with high-speed tissue mashing machine, adds absolute ethyl alcohol 500mL,
35 DEG C, ultrasonic extraction in 300w, 40kHz supersonic wave cleaning machine, extract 1h, filter extract solution, collect filtrate.In triplicate,
Merge all filtrates.Filtrate is evaporated to dryness in Rotary Evaporators, revolving temperature is 30 DEG C, and revolving residue is dissolved in
In 10ml absolute ethyl alcohols, the crude extract 1.23mg/g of glycerine is obtained.
Precision weighs 1.000mg glycerine standard items and is dissolved in 1.0mL methanol, obtains the glycerine standard items that concentration is 1mg/mL
Solution.
By sample liquid and standard items liquid point in (5 × 10cm on same High Performance Thin silica gel H plate2) on, solvent volume
Than for dichloromethane:Methanol=5:1, solvent is added into expansion cylinder (10 × 12 × 15cm3), pre-equilibration 30min at room temperature,
High Performance Thin plate is placed into, when exhibition is away from 9cm is reached, expansion terminates, and is dried after plate is deployed.Dyed, used with alkalinity potassium permanganate
Hair-dryer heating 2min (70 DEG C), under purple background, glycerine displaing yellow.Dual wavelength is carried out with CAMAG thin-layer chromatogram scanners-III
Scanning, Detection wavelength 276nm, reference wavelength 550nm, passes through standard items and the scanning peak area quantification of sample.Obtain drying south
The content of glycerine is 1.21mg/g in the krill of pole..
Embodiment 3
The krill 40g of freeze-drying is taken, is crushed with high-speed tissue mashing machine, adds absolute ethyl alcohol 400mL,
35 DEG C, ultrasonic extraction in 300w, 40kHz supersonic wave cleaning machine, extract 1h, filter extract solution, collect filtrate.In triplicate,
Merge all filtrates.Filtrate is evaporated to dryness in Rotary Evaporators, revolving temperature is 50 DEG C, and revolving residue is dissolved in
In 10ml absolute ethyl alcohols, the crude extract of glycerine is obtained.
Precision weighs 1.000mg glycerine standard items and is dissolved in 1.0mL methanol, obtains the glycerine standard items that concentration is 1mg/mL
Solution.
By sample liquid and standard items liquid point in (5 × 10cm on same High Performance Thin silica gel H plate2) on, solvent volume
Than for dichloromethane:Methanol=5:1, solvent is added into expansion cylinder (10 × 12 × 15cm3), pre-equilibration 30min at room temperature,
High Performance Thin plate is placed into, when exhibition is away from 9cm is reached, expansion terminates, and is dried after plate is deployed.Dyed, used with alkalinity potassium permanganate
Hair-dryer heating 3min (60 DEG C), under purple background, glycerine displaing yellow.Dual wavelength is carried out with CAMAG thin-layer chromatogram scanners-III
Scanning, Detection wavelength 276nm, reference wavelength 550nm, passes through standard items and the scanning peak area quantification of sample.Obtain drying south
The content of glycerine is 1.18mg/g in the krill of pole.
The High Performance Thin double-wavelength scan detection method of present invention detection krill glycerine, the detection of its glycerine thin-layer chromatography
Standard curve to establish mode as follows:
(1) precision, which weighs 1.0000mg glycerine standard items (Sigma companies) and is dissolved in, obtains concentration in 1.0mL methanol and is
1.0mg/mL titer;
(2) the good glycerine titer of above-mentioned configuration 2 μ L are taken, 2.5 μ L, 3.5 μ L, 4 μ L, 4.5 μ L, point sample is efficient in same
Thin layer silica gel H plate, deploy according to the unfolding condition of glycerine, dry.
(3) after being dyed with alkalinity potassium permanganate, with CAMAG thin-layer chromatogram scanner-III, Detection wavelength 276nm, reference wavelength
550nm carries out double-wavelength scan detection, through thin layer scanning software Wincats 1.4.1 statistics (table 1), obtains regression equation
Y=-7025.028+6167.319 × X, r=0.99928, sdv=2.10%.
Table 1:
Point sample amount (μ g) | Peak area (AU) |
2 | 5339.70 |
2.5 | 8492.91 |
3.5 | 14160.25 |
4 | 17895.91 |
4.5 | 20746.85 |
The High Performance Thin double-wavelength scan detection method of present invention detection krill glycerine, it is its precision, repeatability, steady
It is qualitative, rate of recovery situation is as follows:
1. precision determines
Precision draws standard items liquid, the horizontal μ L of point sample 2.5 on same High Performance Thin silica gel plate, expansion, dries, uses alkali
CAMAG thin-layer chromatogram scanner-III are used after property potassium permanganate stain, with 276nm, 550nm double-wavelength scans peak area such as following table (table
2):
Table 2:
Point | 1 | 2 | 3 | 4 | 5 | RSD |
Peak area (AU) | 8582.6 | 8504.4 | 8596.3 | 8454.8 | 8649.5 | 0.9% |
2. repeatability measure
Precision draws standard items liquid, and the μ L of point sample 2.5 are distinguished on 5 blocks of High Performance Thin silica gel plates, expansion, are dried, with alkalescence
CAMAG thin-layer chromatogram scanner-III are used after the dyeing of potassium permanganate developer, with 276nm, 500nm absorbing wavelengths scanning peak area is as follows
Table (table 3).
Table 3:
Plate | 1 | 2 | 3 | 4 | 5 | RSD |
Peak area (AU) | 8402.7 | 8438.0 | 8459.5 | 8673.5 | 8599.0 | 1.36% |
3. Stability Determination
Precision draws horizontal 3 points of point sample of μ L of standard items liquid 2.5 on High Performance Thin plate, expansion, dries, alkaline permanganic acid
CAMAG thin-layer chromatogram scanner-III are used after potassium dyeing, with 276nm, 550nm absorbing wavelengths scanning, later every 1h run-downs, note
Each peak area is recorded, calculates corresponding RSD, test of many times proves, more stable in 0-2h after dyeing, average RSD=
0.77%, specific data are shown in Table 4.
Table 4:
4. recovery test
Precision draws 3 μ L samples liquid 3 times, is separately added into, and 1.82 μ g, 3.64 μ g, 5.46 μ g glycerine standard items, point sample, opens up
Open, dry, with CAMAG thin-layer chromatogram scanner-III are used after alkalinity potassium permanganate staining reagent, with 276nm, 550nm absorbing wavelengths
Scanning, calculate average recovery rate is 97.2%, RSD=1.4%.Data are as shown in table 5:
Table 5:
Sample size/μ g | Add standard items amount/μ g | Measured amount/μ g | Rate of recovery % |
2.90 | 1.45 | 4.28 | 98.4% |
2.90 | 2.90 | 5.65 | 97.4% |
2.90 | 4.35 | 6.94 | 95.7% |
The preferred embodiment of the application is the foregoing is only, is not limited to the application, for the skill of this area
For art personnel, the application can have various modifications and variations.It is all within spirit herein and principle, made any repair
Change, equivalent substitution, improvement etc., should be included within the protection domain of the application.
Claims (10)
1. the method for glycerine, its feature exist in a kind of dual wavelength thin-layer chromatography scanning quantitation analysis krill glycerine crude extract
In step includes:
1) glycerine standard items are dissolved in methanol, standard items liquid is made;
2) using glycerine crude extract as sample liquid and standard items liquid spotting in same thin layer silica gel H plate, with dichloromethane:Methanol
=5:1 is solvent, pre-equilibration 20-30min, thin-layer developing;
3) after expansion terminates, thin layer silica gel plate is taken, is dried, dyed;
4) thin-layer chromatogram scanner carries out double-wavelength scan, passes through examination criteria product liquid and the scanning integrating peak areas value of sample liquid, meter
Calculation obtains glycerol content in krill glycerine crude extract.
2. a kind of analysis method as claimed in claim 1, it is characterised in that in step 1), the concentration of the standard items liquid is
1mg/ml。
3. a kind of analysis method as claimed in claim 1, it is characterised in that in step 2), thin-layer developing exhibition is away from for 8~10cm
(being preferably 9cm).
4. a kind of analysis method as claimed in claim 1, it is characterised in that in step 3), with alkalinity potassium permanganate developer
Plate dyeing is sprayed, is then toasted 2~3 minutes at 60~70 DEG C.
5. a kind of analysis method as claimed in claim 1, it is characterised in that in step 4), dual wavelength parameter is specially to detect
Wavelength 276nm, reference wavelength 550nm.
6. a kind of analysis method as claimed in claim 1, it is characterised in that in step 4), with the quality (μ of glycerine standard items
G) it is abscissa (X), integrating peak areas value (AU) is ordinate (Y), and it is Y=-7025.028+6167.319 to obtain regression equation
× X, r=0.99928.
A kind of 7. analysis method as claimed in claim 1, it is characterised in that the preparation side of the krill glycerine crude extract
Method is:
Fresh krill and absolute ethyl alcohol are pressed into mass volume ratio 1g:(10-15) ml is mixed, and ultrasonic extraction, filtrate is evaporated,
Glycerine crude extract is dissolved to obtain with absolute ethyl alcohol.
8. a kind of analysis method as claimed in claim 1, it is characterised in that the condition of the ultrasonic extraction is:30~40 DEG C,
250~350W, 30~50kHz, extraction time are 0.8~1.5h.
9. a kind of analysis method as claimed in claim 8, it is characterised in that the condition of the ultrasonic extraction is:35℃、
300W, 40kHz, extraction time 1h, in triplicate, collect filtrate.
10. any one of the claim 1-9 analysis methods answering in glycerine in quantitative determining krill glycerine crude extract
With.
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CN105067736A (en) * | 2015-07-23 | 2015-11-18 | 山东师范大学 | Method for extracting and detecting glycerol from Euphausia superba |
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