CN105067736A - Method for extracting and detecting glycerol from Euphausia superba - Google Patents
Method for extracting and detecting glycerol from Euphausia superba Download PDFInfo
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- CN105067736A CN105067736A CN201510439899.1A CN201510439899A CN105067736A CN 105067736 A CN105067736 A CN 105067736A CN 201510439899 A CN201510439899 A CN 201510439899A CN 105067736 A CN105067736 A CN 105067736A
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Abstract
The present invention discloses a method for extracting and detecting glycerol from Euphausia superba. The method comprises: (1) adopting Euphausia superba as a raw material, adopting ethanol as a solvent, carrying out ultrasonic extraction, and filtering the extraction solution to obtain the filtrate; (2) evaporating the filtrate to obtain a crude extract of the glycerol; (3) refining the crude extract of the glycerol by using column chromatography; (4) carrying out primary detection to obtain a glycerol sample; and (5) further detecting the glycerol by using gas chromatography-mass spectrometry, and calculating the content. According to the present invention, the operations of the extraction method is simple, accurate and reliable, the complete method is provided for the extraction and the detection of the glycerol from the Euphausia superba; and with the method, the utilization value of the Euphausia superba is further developed, and the direction is provided for the clean renewable energy sources.
Description
Technical field
The present invention relates to a kind of method of isolation and determination glycerine from krill, belong to food and chemical field.
Background technology
Glycerinated formal name used at school is glycerine, is conventional a kind of organic multicomponent alcoholic compound.Taking glycerine as raw material, can multiple deep processing be carried out, preparing the multiple converted products such as epichlorokydrin, 1,2-PD, 1,3-PD, glyceryl tertbutyl ether, carbonic acid glyceride as utilized glycerine.The cryoprotectant of glycerine Chang Zuowei cell, has anti-cold effect; The discovery of glycerine in krill body, may to adapt to South Pole cold climate relevant with krill, is conducive to existence and the physiological activity of krill; The glycerine simultaneously extracted from krill can be used for the development of cold-resistant material, cosmetics, skin care item.
Krill is a kind of important living resources in Antarctic ecosystems, belongs to Arthropoda, Crustachia, Euphausiacea, and the bodily form like shrimp, is the main food source of the Antarctic organisms such as marine mammal, birds and fish.According to statistics, the quantity of living in the krill in the waters, the Antarctica of Antarctic Ocean can reach 2 × 10
9ton, possible quantity of the catch is estimated 5 × 10
6to 7 × 10
6ton.The life-span of krill is generally 5-7, and namely ripe after 2 ages, body length is maximum reaches more than 60nm.Krill has the habit of knot group, and the shoaling layer through about the 200m that is everlasting forms intensive colony.Because krill has, biomass is large, distribute the feature such as wide, and increasing researcher starts the value of exploiting and utilizing paying close attention to krill.
Glycerine is mainly extensively present in occurring in nature with the form of glyceride.So for a long time, most of glycerine produces soap from fat saponification and produce the process of fatty acid from grease hydrolysis to obtain as accessory substance.1858, people know also can glycerine processed with fermentation method.From 1948, started industrially to apply by the method for propylene synthetic glycerine, output rose year by year, and development trend is very fast.Now, the industrial process of glycerine can be divided into 3 classes by the source of glycerine, i.e. the production of natural glycerin, the production of fermentation glycerol, the production of synthetic glycerine.
The shortcoming of the technique of chemical method synthetic glycerine is: will day by day consuming of the non-renewable energy resources such as oil, and the chemical solvent contaminated environment used in production run, produces a large amount of waste water, waste residue etc., and the glycerine of chemosynthesis, unsuitable skin care, medical.And the shortcoming of the technique of fermenting and producing glycerine to be fermentation period long, it is low to produce glycerine rate, natural glycerin and fermentation glycerol, suitable medical, change shape product and use;
From krill, do not extract the relevant report of glycerine at present, more there is no the method for isolation and determination glycerine from krill.
Summary of the invention
The object of this invention is to provide a kind of method of isolation and determination glycerine from krill, the method is simple to operate, accurate and reliable.
The present invention is achieved by the following technical solutions:
From krill, extract a method for glycerine, comprise the following steps:
(1) take krill as raw material, employing ethanol is solvent, 20-40 DEG C, ultrasonic extraction under the condition of 300-400W, 20-40kH, filters extract, obtains filtrate;
(2) by filtrate evaporate to dryness, the crude extract of glycerine is obtained;
(3) crude extract of column chromatography to glycerine is utilized to refine:
1. silica gel column chromatography is prepared;
2. the crude extract of glycerine is joined on silica gel bed;
3. wash-out: eluant, eluent is the mixed solution of methylene chloride and methyl alcohol, controls elution volume, collects the eluent of 600 ~ 900mL, and eluent is concentrated, dry, obtain glycerine.
From krill, detect a method for glycerine, comprise the following steps:
(1) take krill as raw material, employing ethanol is solvent, 20-40 DEG C, ultrasonic extraction under the condition of 300-400W, 20-40kH, filters extract, obtains filtrate;
(2) by filtrate evaporate to dryness, the crude extract of glycerine is obtained;
(3) crude extract of column chromatography to glycerine is utilized to refine:
1. silica gel column chromatography is prepared;
2. the crude extract of glycerine is joined on silica gel bed;
3. wash-out: eluant, eluent is the mixed solution of methylene chloride and methyl alcohol, controls elution volume, Fractional Collections eluent, collects several times, and eluent is concentrated, dry, obtain some parts of sample liquid;
(4) Preliminary detection glycerine:
Get some parts of sample liquid and carry out TLC Preliminary detection, by some parts of sample liquid points on High Performance Thin silica gel plate, take volume ratio as methylene chloride: methyl alcohol=3 ~ 4:1 is developping agent, launch in exhibition cylinder, exhibition is apart from being 8 ~ 10cm (being preferably 9cm), panel is dried after having opened up, use anisaldehyde staining reagent, toast 6-10 minute at being then placed in 100-105 DEG C, according to color, select color to be changed to green sample liquid, be glycerine.
(5) gas chromatography-mass spectrum is adopted to detect glycerine further:
Gas chromatography-mass spectrum testing conditions: (volume ratio of preferred cyanogen propyl group phenyl and dimethyl polysiloxane is 6:94 to adopt cyanogen propyl group phenyl-dimethyl polysiloxane mixed solution,) be the capillary column of immobile liquid, temperature programme, initial temperature is 100 DEG C, maintain 4 minutes, with the ramp to 120 DEG C of 50 DEG C per minute, maintain 10 minutes, again with the ramp to 220 DEG C of 50 DEG C per minute, maintain 6 minutes; Injector temperature is 200 DEG C; Detector temperature is 250 DEG C.Ionization mode: electron bombardment ionization source (EI), level Four bar temperature 150 DEG C, ion source temperature 230 DEG C; Monitoring mode: full surface sweeping (50-550amu unit); Selective ion mode scan pattern (SIM); Ionizing energy: 70eV; Solvent delay: 2min;
Obtain sample matter collection of illustrative plates, determining that color is changed to green sample liquid is glycerine, and calculates the content of glycerine.
In step (1), described krill water cut is 7 ~ 8%, and the addition ratio of krill and ethanol is: 1g:(5 ~ 10) mL.Prove through a large amount of experiments, when the mass volume ratio of krill and ethanol is 1g:(5 ~ 10) mL time, the extraction effect of glycerine sample is best.
In step (1), described ethanol to be massfraction be 95% ethanolic solution.
In step (2), concrete operation steps is: filtrate being placed in step (1) revolved and steam instrument, and in order to prevent high temperature from making glycerine go bad, evaporate to dryness under 35 DEG C of conditions, obtains the crude extract of glycerine.
Step (3) 1. in, the concrete grammar preparing silica gel column chromatography is:
Get 60-70g, 200-300 order silica gel and at 100-110 DEG C, activate 8-10 hour, cool to room temperature; Add 2-3 times of volumes methylene chloride to stir, make silica gel suspend into pasty state homogenate; Chromatographic column cock is opened, silica-dichloromethane potpourri is gently poured in chromatographic column along glass bar, knock chromatographic column tube wall gently with ear washing bulb and drive bubble, knock while drip methylene chloride until the complete sedimentation of silicagel column; When methylene chloride liquid level arrives silica gel bed surface just, cut-out tap.
Step (3) 2. in, concrete grammar is: slowly drip on silica gel bed surface along chromatographic column tube wall by glycerine crude extract with glue head dropper, notes reducing disturbance to bed surface.Open cock, make sample slowly enter end face, then use 1-2mL washed with dichloromethane top post jamb.
Step (3) 3. in, described methylene chloride and methyl alcohol volume ratio are 8:1.Adopt the eluent efficiency of this ratio high, elution time is short.
Control elution volume, every 250 ~ 300mL collects an eluent, and collect several times, collection frequence is greater than 3 times, and eluent is concentrated, dry, obtain some parts of sample liquid.Adopt this kind of method, the collection of eluent and follow-up detection efficiency are all improved.
One preferably elution process is: when sample liquid level arrives silica gel bed end face just, add eluant, eluent and start wash-out; Be methylene chloride by volume ratio: the eluent of methyl alcohol=8:1 carries out wash-out, control elution volume, every 300mL collects an eluent, collects 3 times, numbering 1-3, and eluent is concentrated, drying, obtain 3 parts of sample liquid.Through lot of experiment validation, every 300mL collects an eluent, and the eluent when collecting for the 3rd time can obtain the whole glycerine in crude extract.
In step (4), the model of described High Performance Thin silica gel plate is GF
254, investigate the High Performance Thin silica gel plate of different model, obtaining model is GF
254high Performance Thin silica gel plate separating effect best.
The invention has the beneficial effects as follows:
Method of the present invention is simple to operate, accurate, environmental protection and reliable, extracts the glycerine purity obtained very high, for krill isolation and determination glycerine provides complete method.After testing and to calculate glycerol content in krill be 1.51mg/g.
The present invention is isolation and determination glycerine from krill, further developed the value of krill, simultaneously also for clean renewable energy utilization provider to.
Accompanying drawing explanation
Fig. 1: A is the gas chromatography retention time image of sample in embodiment 1; B is the gas chromatography retention time image of embodiment 1 Plays product.
Fig. 2: A is the mass spectrogram of sample in embodiment 1; B is the mass spectrogram of embodiment 1 Plays product.
Fig. 3: A is the gas chromatography retention time image of sample in embodiment 2; B is the gas chromatography retention time image of embodiment 2 Plays product.
Fig. 4: A is the mass spectrogram of sample in embodiment 2; B is the mass spectrogram of embodiment 2 Plays product.
Fig. 5: A is the gas chromatography retention time image of sample in embodiment 3; B is the gas chromatography retention time image of embodiment 3 Plays product.
Fig. 6: A is the mass spectrogram of sample in embodiment 3; B is the mass spectrogram of embodiment 3 Plays product.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further described.
Embodiment 1
Get dry krill 2g, be placed in 200mL, diameter is the beaker of 6cm, adding massfraction is 95% ethanol 10mL, in room temperature, the ultrasonic extraction of 350W, 40kHz, extract 10 minutes, filter extract, filtrate being placed in is revolved and steams instrument 35 DEG C of evaporates to dryness, obtain the crude extract of glycerine.
Get 60g, 200 ~ 300 order silica gel 100 DEG C of activation 10 hours, be cooled to room temperature; Add silica gel 2 times of volumes methylene chloride to stir, make silica gel suspend into pasty state homogenate; Chromatographic column cock is opened, silica-dichloromethane potpourri is gently poured in chromatographic column along glass bar, knock chromatographic column tube wall gently with ear washing bulb and drive bubble, knock while drip methylene chloride until the complete sedimentation of silica gel; When methylene chloride liquid level arrives silica gel bed surface just, cut-out tap.Along chromatographic column tube wall, glycerine crude extract is slowly dripped on silica gel bed surface with glue head dropper, note reducing the disturbance to bed surface.Opening cock, is that sample slowly enters end face, then uses 1mL washed with dichloromethane top post jamb, when liquid level arrives silica gel bed end face just, adds eluant, eluent and starts wash-out; With methylene chloride: methyl alcohol 8:1 (volume ratio) carries out wash-out, control elution volume, every 300mL collects an eluent, collects 5 times, numbering 1-5, and eluent is concentrated, drying; By No. 3 sample liquid 5ul points in GF
254on High Performance Thin silica gel plate, take volume ratio as methylene chloride: methyl alcohol=3:1 is developping agent, launch in exhibition cylinder, exhibition, apart from being 9cm, being dried panel after having opened up, is used anisaldehyde staining reagent, toasts 10 minutes, carry out Preliminary detection at being then placed in 100 DEG C; Utilize gas chromatograph-mass spectrometer (GCMS), with the capillary column of massfraction be 6% cyanogen propyl group phenyl-massfraction to be 94% dimethyl polysiloxane be immobile liquid, temperature programme, initial temperature is 100 DEG C, maintain 4 minutes, with the ramp to 120 DEG C of 50 DEG C per minute, maintain 10 minutes, again with the ramp to 220 DEG C of 50 DEG C per minute, maintain 6 minutes; Injector temperature is 200 DEG C; Detector temperature is 250 DEG C.Ionization mode: electron bombardment ionization source (EI), level Four bar temperature 150 DEG C, ion source temperature 230 DEG C; Monitoring mode: full surface sweeping (50-550amu unit); Selective ion mode scan pattern (SIM); Ionizing energy: 70eV; Solvent delay: 2min; Detect according to above detection method, obtain detection figure, as Fig. 1 and 2.After testing and to calculate glycerol content in krill be 1.51mg/g.
Embodiment 2
Get dry krill 2g, be placed in 200mL, diameter is the beaker of 6cm, add 95% ethanol 15mL, in room temperature, the ultrasonic extraction of 350w, 28kHz, extract 15 minutes, filter extract, filtrate being placed in is revolved and steams instrument 35 DEG C of evaporates to dryness, obtain the crude extract of glycerine.
Get 65g, 200-300 order silica gel and activate 9 hours at 105 DEG C, be cooled to room temperature; Add 2 times of volumes methylene chloride to stir, make silica gel suspend into pasty state homogenate; Chromatographic column cock is opened, silica-dichloromethane potpourri is gently poured in chromatographic column along glass bar, knock chromatographic column tube wall gently with ear washing bulb and drive bubble, knock while drip methylene chloride until the complete sedimentation of silicagel column; When methylene chloride liquid level arrives silica gel bed surface just, cut-out tap.Along chromatographic column tube wall, glycerine crude extract is slowly dripped on silica gel bed surface with glue head dropper, note reducing the disturbance to bed surface.Open cock, make sample slowly enter end face, then use 1mL washed with dichloromethane top post jamb, when liquid level arrives silica gel bed end face just, add eluant, eluent and start wash-out; With methylene chloride: methyl alcohol 8:1 (volume ratio) carries out wash-out, control elution volume, every 300mL collects an eluent, collects 5 times, numbering 1-5, and eluent is concentrated, drying; By No. 3 sample liquid 5ul points in GF
254on High Performance Thin silica gel plate, take volume ratio as methylene chloride: methyl alcohol=4:1 is developping agent, launch in exhibition cylinder, exhibition, apart from being 9cm, being dried panel after having opened up, is used anisaldehyde staining reagent, toasts 8 minutes, carry out Preliminary detection at being then placed in 105 DEG C; Detect according to the method in embodiment 1, obtain detection figure, as Fig. 3 and 4.After testing and to calculate glycerol content in krill be 1.51mg/g.
Embodiment 3
Get dry krill 2g, be placed in 200mL, diameter is the beaker of 6cm, add 95% ethanol 20mL, in room temperature, the ultrasonic extraction of 350w, 20kHz, extract 15 minutes, filter extract, filtrate being placed in is revolved and steams instrument 35 DEG C of evaporates to dryness, obtain the crude extract of glycerine.
Get 70g, 200-300 order silica gel and activate 8 hours at 110 DEG C, be cooled to room temperature; Add 2 times of volumes methylene chloride to stir, make silica gel suspend into pasty state homogenate; Chromatographic column cock is opened, silica-dichloromethane potpourri is gently poured in chromatographic column along glass bar, knock chromatographic column tube wall gently with ear washing bulb and drive bubble, knock while drip methylene chloride until the complete sedimentation of silicagel column; When methylene chloride liquid level arrives silica gel bed surface just, cut-out tap.Along chromatographic column tube wall, glycerine crude extract is slowly dripped on silica gel bed surface with glue head dropper, note reducing the disturbance to bed surface.Open cock, make sample slowly enter end face, then use 1mL washed with dichloromethane top post jamb, when liquid level arrives silica gel bed end face just, add eluant, eluent and start wash-out; With methylene chloride: methyl alcohol 8:1 (volume ratio) carries out wash-out, control elution volume, every 300mL collects an eluent, collects 5 times, numbering 1-5, and eluent is concentrated, drying; By No. 3 sample liquid 5ul points in GF
254on High Performance Thin silica gel plate, take volume ratio as methylene chloride: methyl alcohol=4:1 is developping agent, launch in exhibition cylinder, exhibition, apart from being 9cm, being dried panel after having opened up, is used anisaldehyde staining reagent, toasts 6 minutes, carry out Preliminary detection at being then placed in 110 DEG C; Detect according to the method in embodiment 1, obtain detection figure, as Fig. 5 and 6.After testing and to calculate glycerol content in krill be 1.5mg/g.
By reference to the accompanying drawings the specific embodiment of the present invention is described although above-mentioned; but not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendment or distortion that creative work can make still within protection scope of the present invention.
Claims (9)
1. from krill, extract a method for glycerine, it is characterized in that, comprise the following steps:
(1) take krill as raw material, employing ethanol is solvent, 20-40 DEG C, 300-400W ,/20-40kHz condition under ultrasonic extraction, filter extract, obtain filtrate;
(2) by filtrate evaporate to dryness, the crude extract of glycerine is obtained;
(3) crude extract of column chromatography to glycerine is utilized to refine:
1. silica gel column chromatography is prepared; 2. the crude extract of glycerine is joined on silica gel bed;
3. wash-out: eluant, eluent is the mixed solution of methylene chloride and methyl alcohol, controls elution volume, collects the eluent of 600 ~ 900mL, and eluent is concentrated, dry, obtain glycerine.
2. the method for claim 1, is characterized in that: in step (1), and the addition ratio of krill and ethanol is: 1g:(5 ~ 10) mL.
3. the method for claim 1, is characterized in that: in step (2), by filtrate evaporate to dryness under 35 DEG C of conditions, obtain the crude extract of glycerine.
4. the method for claim 1, is characterized in that: in step (3), and described methylene chloride and methyl alcohol volume ratio are 8:1.
5. detect a method for glycerine in krill, it is characterized in that, comprise the following steps:
(1) take krill as raw material, employing ethanol is solvent, 20-40 DEG C, ultrasonic extraction under the condition of 300-400W, 20-40kHz, filters extract, obtains filtrate;
(2) by filtrate evaporate to dryness, the crude extract of glycerine is obtained;
(3) crude extract of column chromatography to glycerine is utilized to refine:
1. silica gel column chromatography is prepared; 2. the crude extract of glycerine is joined on silica gel bed;
3. wash-out: eluant, eluent is the mixed solution of methylene chloride and methyl alcohol, controls elution volume, Fractional Collections eluent, collects several times, and eluent is concentrated, dry, obtain some parts of sample liquid;
(4) Preliminary detection glycerine:
Get some parts of sample liquid and carry out TLC Preliminary detection, by some parts of sample liquid points on thin-layer silicon offset plate, take volume ratio as methylene chloride: methyl alcohol=3 ~ 4:1 is developping agent, launch in exhibition cylinder, exhibition, apart from being 8 ~ 10cm, dries panel after having opened up, use anisaldehyde staining reagent, then toast 6-10 minute at being placed in 100-105 DEG C, according to color, select color to be changed to green
'ssample liquid, green sample liquid is glycerine.
6. method as claimed in claim 5, is characterized in that: in step (3), and control elution volume, every 250 ~ 300mL collects an eluent, and collect several times, collection frequence is greater than 3 times, and eluent is concentrated, dry, obtain some parts of sample liquid.
7. method as claimed in claim 6, is characterized in that: control elution volume, every 300mL collects an eluent, collects 3 times, and eluent is concentrated, drying, obtain 3 parts of sample liquid.
8. method as claimed in claim 5, is characterized in that: the model of described High Performance Thin silica gel plate is GF
254.
9. method as claimed in claim 5, is characterized in that: also comprise and adopt gas chromatography-mass spectrum to detect glycerine further:
Gas chromatography-mass spectrum testing conditions: the mixed solution adopting cyanogen propyl group phenyl-dimethyl polysiloxane is the capillary column of immobile liquid, temperature programme, initial temperature is 100 DEG C, maintain 4 minutes, with the ramp to 120 DEG C of 50 DEG C per minute, maintain 10 minutes, then with the ramp to 220 DEG C of 50 DEG C per minute, maintain 6 minutes; Injector temperature is 200 DEG C; Detector temperature is 250 DEG C; Ionization mode: electron bombardment ionization source, level Four bar temperature 150 DEG C, ion source temperature 230 DEG C; Monitoring mode: full surface sweeping, 50-550amu unit; Selective ion mode scan pattern; Ionizing energy: 70eV; Solvent delay: 2min;
Obtain sample mass-spectrogram, determining that color is changed to green sample liquid is glycerine, and calculates the content of glycerine.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107607668A (en) * | 2017-08-23 | 2018-01-19 | 山东师范大学 | A kind of method of glycerine in dual wavelength thin-layer chromatography scanning quantitation analysis krill glycerine crude extract |
| CN109632560A (en) * | 2018-12-07 | 2019-04-16 | 北京彤程创展科技有限公司 | The method and its application of oil content are filled in a kind of fast quantification insoluble sulfur |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107607668A (en) * | 2017-08-23 | 2018-01-19 | 山东师范大学 | A kind of method of glycerine in dual wavelength thin-layer chromatography scanning quantitation analysis krill glycerine crude extract |
| CN109632560A (en) * | 2018-12-07 | 2019-04-16 | 北京彤程创展科技有限公司 | The method and its application of oil content are filled in a kind of fast quantification insoluble sulfur |
| CN109632560B (en) * | 2018-12-07 | 2021-06-15 | 北京彤程创展科技有限公司 | Method for rapidly quantifying content of filling oil in insoluble sulfur and application thereof |
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