CN107085069A - A kind of thin-layer sample application method for being used to prepare thin-layer chromatography - Google Patents
A kind of thin-layer sample application method for being used to prepare thin-layer chromatography Download PDFInfo
- Publication number
- CN107085069A CN107085069A CN201710332886.3A CN201710332886A CN107085069A CN 107085069 A CN107085069 A CN 107085069A CN 201710332886 A CN201710332886 A CN 201710332886A CN 107085069 A CN107085069 A CN 107085069A
- Authority
- CN
- China
- Prior art keywords
- sample
- thin
- lamellae
- layer
- point
- 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.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
- G01N30/91—Application of the sample
Abstract
The invention discloses a kind of thin-layer sample application method for being used to prepare thin-layer chromatography.Belong to thin-layer chromatographic analysis and preparing technical field.The inventive method is mainly included the following steps that：The preparation of lamellae, the preparation of spot sample device, point sample, sample expansion and example enrichment.The inventive method has the advantages that equipment is simple, easy to operate, quick and easy, cost is low, good separating effect after sample expansion.
Description
Technical field
The invention belongs to thin-layer chromatographic analysis and preparing technical field, and in particular to a kind of method for preparing thin-layer sample application.
Background technology
Thin-layer chromatography equipment is simple, and easy to operate, wide adaptability can quickly provide reliable, accurate experimental result, be
A kind of alternative economic, reliable, quick analysis method.Conventional thin-layer chromatography volume containing the sample is few, is used for qualitative analysis,
Sample can not be largely prepared, and it is the extension to commonly using thin-layer chromatography application to prepare chromatogram, overcomes conventional thin-layer chromatography load sample
The few shortcoming of amount, had not only remained separating effect rapidly and efficiently but also the effect of preparation can be reached to mixture, with it is easy to operate,
Equipment is simple, analysis prepares fireballing advantage.Although column chromatography is purification of samples common method, for a small amount of to be separated or
Stationary phase in hardly possible separation sample, column chromatography may waste some samples and cost is big, and due to that can not detect in real time, point
It is poor from effect, it is difficult to obtain sterling.Therefore for the preparation of a small amount of sample, it is that a kind of inexpensive, equipment is simple to prepare chromatogram, point
From fireballing effective ways.
Conventional preparation method, on plate is prepared during point sample, commonly uses spot application, wavy bar is presented on lamellae
Band, the so sample for inferior separating effect, the band of multiple compounds are likely to occur intersection, it is difficult to which analysis separates system with sample
It is standby.
The content of the invention
The purpose of the present invention is that there is provided a kind of thin-layer sample application for thin-layer chromatographic analysis in view of the shortcomings of the prior art
Preparation method, method of the invention has that equipment is simple, easy to operate, step is few, quick and easy, and cost is low, and point sample is accurate
Advantage, make a small amount of sample by the present invention method be effectively obtained separation prepare.
The technical solution adopted by the present invention is：A kind of thin-layer sample application method for being used to prepare thin-layer chromatographic analysis, including with
Lower step：
1) preparation of lamellae：Take silica gel and sodium carboxymethyl cellulose solution well mixed, stir and moisten completely to silica gel
It is wet, the bubble in ultrasonically treated 4-5min, fully discharge solution, then by the silica gel modulated in being smoothened on glass plate, room temperature
After lower drying, it is placed in baking oven, in drying 20-40min at 100-110 DEG C, obtains lamellae；
2) preparation of spot sample device：Take glass cement head dropper and absorbent cotton, by absorbent cotton rub into after the long fine strip shapes of 1cm from
The absorbent cotton that 0.4-0.6cm is reserved outside glue head dropper, the lower end port of export is filled in glue head dropper lower end, in writing brush shape；
3) point sample：Scale is put in away from the 1-5cm of lamellae lower end, it is parallel with lamellae lower edge, using pencil along scale
A point line-transect is gently drawn, spot sample device absorbent cotton one end is submerged into sample, appropriate amount of sample is drawn, then at the uniform velocity along point line-transect point
Plate；
4) sample deploys：Mobile phase is prepared, the lamellae after point sample is deployed in chromatography cylinder, is taken out, is dried, put ultraviolet
Inspected under lamp；
5) example enrichment：Scraped along expansion band edge circle with scraper by band is deployed, the sample for being taken expansion with organic solvent
Component dissolves, and filtering, filtrate is concentrated under reduced pressure in Rotary Evaporators, obtains powder sample.
A kind of above-mentioned thin-layer sample application method for being used to prepare thin-layer chromatography, it is characterised in that described glass cement head drop
The a diameter of 2-5mm of the port of export of pipe.
The invention has the advantages that：
1. the present invention, passes through the innovation to spot sample device and point sample mode so that the analysis and preparation of a small amount of sample, operation
More facilitate, and point sample effect is more preferable.
2. the present invention, passes through the innovation to spot sample device and point sample mode so that during point sample, overcome traditional wavy
The defect of lines, point sample mode of the invention makes sample that parallel chromatographic band is presented so that sample separating effect is more preferable, Duo Gehua
The band of compound is not in intersect, and is easy to expansion and sample preparation.
3. prepared by the present invention, qualitative analysis and separation for sample so that analysis process is more efficient, quickly, analysis
As a result it is more accurate.
4. the present invention, relatively low to equipment and cost requirements and easy to operate, step is few, and flexibility is big.
5. the present invention is easy to promote, it may not be necessary to which special installation can carry out the work, for a small amount of or difficult separation sample
Analysis and separation prepare for be a kind of good method.
6. the present invention, prepared spot sample device end is the soft absorbent cotton of material, it can prevent from scratching thin layer during point sample
Plate is so as to preferably in thin layer lining out, beneficial to sample expansion.
Brief description of the drawings
Fig. 1 is the structural representation of spot sample device of the present invention.
Fig. 2 is the partial enlarged drawing of spot sample device of the present invention.
Fig. 3 is the design sketch of conventional point sample.
Fig. 4 is to use spot sample device point sample effect diagram of the present invention.
Embodiment
This patent is by taking white paeony root extract as an example, when carrying out thin-layer chromatographic analysis, by preparing the point sample of thin layer to the present invention
It is described further.
Embodiment 1
White paeony root extract is obtained using the method for prior art.
1) preparation of lamellae
Adhesive sodium carboxymethylcellulose (CMC-Na) 5g is weighed in beaker, distilled water 1L is added, heated on electric furnace
Stir about 30min cools down to being completely dissolved, is made into the 0.5%CMC aqueous solution, standby.Weigh the 0.5% of 40g silica gel and 70mL
The CMC aqueous solution, is well mixed, is stirred continuously, and stands, and is stirred for until all silica gel complete wettings, finally use ultrasonication
Bubble in about 4-5min, fully discharge solution.The silica gel modulated is being poured on a piece of 20cm × 20cm just using spoon of horn
In square glass plate, smoothened, gently shaken to surface flat-satin in desktop with spoon of horn.After drying at room temperature, it is placed in baking oven, 105 DEG C
Heat after 30min, lamellae 5 is made, is put into drier, preserve.
2) preparation of spot sample device
Take the long glass cement head droppers 1 of 100mm of the conventional dried and clean in laboratory, the outlet of described glass cement head dropper
The a diameter of about 3mm in end, wears disposable glove extracting degreasing cotton 2 a little, absorbent cotton is rubbed into after the long fine strip shapes of 1cm, from glue head drop
The absorbent cotton that 0.4cm is reserved outside glue head dropper, the lower end port of export is filled in pipe lower end, in writing brush shape, and spot sample device is made.
3) point sample
The scale of dried and clean is taken to be put in away from the 1.5cm of lamellae lower end, it is parallel with lamellae lower edge, marked using pencil edge
Chi gently draws a point line-transect.Spot sample device absorbent cotton one end is submerged into sample, the slow glue head that unclamps makes absorbent cotton one end simultaneously
All the time in sample liquid level lower end, appropriate amount of sample is drawn, then using spot sample device at the uniform velocity along point line-transect continuity point plate.
4) sample deploys
Solvent, by volume, dichloromethane are prepared with dichloromethane and methanol:Methanol=5:1, by the thin layer after point sample
Plate, which is placed in chromatography cylinder, to deploy, and takes out, dries, put and inspected under uviol lamp (254nm).
As a result as shown in figure 3, conventionally using after capillary point sample 3, after deploying through solvent, in ultraviolet lamp inspection
Depending on being in wavy band 4 to two.As shown in figure 4, using the spot sample device point sample 6 prepared by the present invention, through solvent exhibition
After opening, it can be inspected in uviol lamp to two almost parallel bands 7.By Fig. 3 and Fig. 4 it is clear that for the sample of hardly possible separation
Product, the band using the multiple compounds observed after conventional capillaries point sample intersects, it is difficult to reach that sample is kept completely separate
And purpose prepared by analysis, it is easy to scratch lamellae when in addition using capillary point sample, so as to influence separating effect.And adopt
The spot sample device end prepared with the present invention is the soft absorbent cotton of material, can prevent from scratching lamellae during point sample, and can make sample
Product reach separates and can be subsequently used for the analysis and preparation of sample to greatest extent.
5) example enrichment
Gently mark the profile of expansion band with border along two expansion with pencil, and scraped two expansion bands respectively with scraper
Under, it is placed in two 100mL beakers.Proper amount of methanol ultrasound is added in beaker, the component that the expansion scraped takes fully is dissolved
Sample, then respectively filter the solution in two beakers in the funnel equipped with filter paper, take filtrate to put in Rotary Evaporators and depressurize
Concentration is evaporated, and obtains powder sample.
Claims (2)
1. a kind of thin-layer sample application method for being used to prepare thin-layer chromatography, it is characterised in that comprise the following steps：
1) preparation of lamellae：Take silica gel and sodium carboxymethyl cellulose solution well mixed, stir to silica gel complete wetting, surpass
Bubble in sonication 4-5min, fully discharge solution, then dries the silica gel modulated in being smoothened on glass plate at room temperature
Afterwards, it is placed in baking oven, in drying 20-40min at 100-110 DEG C, obtains lamellae；
2) preparation of spot sample device：Glass cement head dropper and absorbent cotton are taken, absorbent cotton is rubbed into after the long fine strip shapes of 1cm from glue head
The absorbent cotton that 0.4-0.6cm is reserved outside glue head dropper, the lower end port of export is filled in dropper lower end, in writing brush shape, and spot sample device is made；
3) point sample：Scale is put in away from the 1-5cm of lamellae lower end, it is parallel with lamellae lower edge, using pencil along scale gently
A point line-transect is drawn, spot sample device absorbent cotton one end is immersed in sample, appropriate amount of sample is drawn, then at the uniform velocity along point line-transect point
Plate；
4) sample deploys：Mobile phase is prepared, the lamellae after point sample is deployed in chromatography cylinder, is taken out, is dried, put under uviol lamp
Inspect；
5) example enrichment：Scraped along expansion band edge circle with scraper by band is deployed, the sample component for being taken expansion with organic solvent
Dissolving, filtering, filtrate is concentrated under reduced pressure in Rotary Evaporators, obtains powder sample.
2. a kind of thin-layer sample application method for being used to prepare thin-layer chromatography according to claim 1, it is characterised in that described
The a diameter of 2-5mm of the port of export of glass cement head dropper.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710332886.3A CN107085069A (en) | 2017-05-12 | 2017-05-12 | A kind of thin-layer sample application method for being used to prepare thin-layer chromatography |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710332886.3A CN107085069A (en) | 2017-05-12 | 2017-05-12 | A kind of thin-layer sample application method for being used to prepare thin-layer chromatography |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107085069A true CN107085069A (en) | 2017-08-22 |
Family
ID=59611899
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710332886.3A Pending CN107085069A (en) | 2017-05-12 | 2017-05-12 | A kind of thin-layer sample application method for being used to prepare thin-layer chromatography |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107085069A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113406262A (en) * | 2021-05-28 | 2021-09-17 | 华南理工大学 | Sample application pen for preparing thin-layer chromatography and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090104686A1 (en) * | 2007-10-21 | 2009-04-23 | King Car Food Industrial Co., Ltd. | Apparatus for Thin-Layer Cell Smear Preparation and In-situ Hybridization |
| CN105294695A (en) * | 2015-09-17 | 2016-02-03 | 中国农业大学 | Compound separated from evodia fargesii dode and insect-resisting application thereof |
| CN105588871A (en) * | 2016-01-14 | 2016-05-18 | 中国检验检疫科学研究院 | Rapid detection method for forbidden Sudan dyes in eye shadow or pressed powder |
-
2017
- 2017-05-12 CN CN201710332886.3A patent/CN107085069A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090104686A1 (en) * | 2007-10-21 | 2009-04-23 | King Car Food Industrial Co., Ltd. | Apparatus for Thin-Layer Cell Smear Preparation and In-situ Hybridization |
| CN105294695A (en) * | 2015-09-17 | 2016-02-03 | 中国农业大学 | Compound separated from evodia fargesii dode and insect-resisting application thereof |
| CN105588871A (en) * | 2016-01-14 | 2016-05-18 | 中国检验检疫科学研究院 | Rapid detection method for forbidden Sudan dyes in eye shadow or pressed powder |
Non-Patent Citations (5)
| Title |
|---|
| BJZHUXIAOBO、QQQ169: "《小木虫论坛 http：//muchong.com/html/200807/879735.html》", 4 July 2008 * |
| 李艳: "楸皮的化学成分及抗肿瘤活性研究", 《中国优秀硕士学位论文全文数据库 医药卫生科技辑》 * |
| 温瑞兴 等: "《药理学实验教程》", 31 May 2014 * |
| 蒋达洪 等: "化学选择性的研究性实验教学：1-苯基丁-3-烯-1-酮的制备", 《化工高等教育》 * |
| 蒋达洪 等: "绿色合成1-苯基丁-3-烯-1-酮实验的微型化研究", 《实验技术与管理》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113406262A (en) * | 2021-05-28 | 2021-09-17 | 华南理工大学 | Sample application pen for preparing thin-layer chromatography and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zarghampour et al. | Simultaneous extraction of acidic and basic drugs via on-chip electromembrane extraction using a single-compartment microfluidic device | |
| RU2013155201A (en) | METHOD FOR TREATING CELLULOSE AND CELLULOSE TREATED ACCORDING TO SUCH METHOD | |
| CN107085069A (en) | A kind of thin-layer sample application method for being used to prepare thin-layer chromatography | |
| Saha et al. | Modern extraction techniques for drugs and medicinal agents | |
| CN102166434B (en) | Mesoporous material coating based open-tubular capillary chromatographic column and preparation method thereof | |
| CN103611501A (en) | Preparation method of polypropylene film micro-solid phase extraction bag based on ZIF-8 adsorbent | |
| MX2012001531A (en) | Method of preparation of samples for analysis and cartridge therefor. | |
| CN105618015B (en) | A kind of preparation of three-dimensional meso-hole carbon composite and its application as solid phase micro-extraction fabric coating material | |
| CN211303747U (en) | Manual box type sample washing and drying instrument | |
| CN103599764A (en) | Preparation method of non-woven fabric micro solid phase extraction (SPE) bag based on ZIF-8 adsorbent | |
| Hashemi et al. | Preparation of a New Solid‐Phase Microextraction Fiber by Coating Silylated Nanoporous Silica on a Copper Wire | |
| CN103611510A (en) | Preparation method of non-woven fabric micro-solid phase extraction bag based on MIL-101 adsorbent | |
| CN104849370A (en) | Method for enrichment analysis of phenolic substances in plant oil based on filter paper-loaded bendazol solid-phase microextraction membrane | |
| JP2015049158A (en) | Absorption pad | |
| CN104628501A (en) | Method for separating and preparing diaryl heptane compounds in walnut green seedcase | |
| CN105067736B (en) | Method for extracting and detecting glycerol from Euphausia superba | |
| CN202555308U (en) | Enclosed water bath heating device | |
| JP5553402B2 (en) | Solid catalyst and method for producing the same | |
| CN204849474U (en) | Papermaking stoving glueing equipment | |
| CN112326863A (en) | Simple preparation plate for thin-layer chromatography separation and using method | |
| CN108627606B (en) | Thin layer identification method of pogostemon cablin | |
| CN104774146B (en) | A kind of preparation method of 7-carbonyl-8,15-isodextropimaric acid methyl ester | |
| CN100488592C (en) | Solid-phase extracting disk of single-wall carbon nano-tube substrate | |
| CN106367325B (en) | Exfoliated cell extractor and the extracting method for utilizing its extraction cast-off cells | |
| CN208161920U (en) | A kind of sizing applicator removes adhesive dispenser |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170822 |
|
| RJ01 | Rejection of invention patent application after publication |