CN204924760U - Chromatography purifying column of well volume sample extract - Google Patents

Chromatography purifying column of well volume sample extract Download PDF

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Publication number
CN204924760U
CN204924760U CN201520682243.8U CN201520682243U CN204924760U CN 204924760 U CN204924760 U CN 204924760U CN 201520682243 U CN201520682243 U CN 201520682243U CN 204924760 U CN204924760 U CN 204924760U
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CN
China
Prior art keywords
splendid attire
cleanser
pipe
glass
decontaminating column
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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
Application number
CN201520682243.8U
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Chinese (zh)
Inventor
孔祥吉
王霞
张雪梅
吴文铸
孔德洋
许静
单正军
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Nanjing Institute of Environmental Sciences MEP
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Nanjing Institute of Environmental Sciences MEP
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Priority to CN201520682243.8U priority Critical patent/CN204924760U/en
Application granted granted Critical
Publication of CN204924760U publication Critical patent/CN204924760U/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

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Abstract

The utility model discloses a chromatography purifying column of well volume sample extract, decontaminating agent splendid attire pipe top tube and decontaminating agent splendid attire pipe low tube including from the top down interconnect, decontaminating agent splendid attire pipe top tube from the top down be application of sample portion, dilatation portion and connecting portion in proper order, wherein, the internal diameter of application of sample portion, dilatation portion and connecting portion than be 4: 5-6: 3, length than be 1: 3-4: 5, upper end in dilatation portion is provided with glass crotch down, lower extreme at connecting portion is provided with upwards curved glass crotch, and the upper end of decontaminating agent splendid attire pipe low tube is provided with the glass crotch to the reclination, and the lower extreme has the activity cock, the quartz sand gasket has been inlayed to the upper end of decontaminating agent splendid attire pipe low tube, decontaminating agent splendid attire pipe top tube and decontaminating agent splendid attire pipe low tube cup joint each other and constitute chromatography purifying column. The utility model discloses main to the operation of the purification in well volume sample extract, have the leakproofness good, can dismantle, prevent shortly to flow, the easy washing, economy is high -efficient, characteristics that the range of application is wide.

Description

A kind of chromatography decontaminating column of middle volume sample extract
Technical field
The utility model relates to a kind of fluid sample pretreating device, relates to a kind of chromatography decontaminating column of middle volume sample extract particularly.
Background technology
The purification run of the organic extract of current environmental sample relies on commercial decontaminating column to complete, as C mostly 18post, nh 2 column, cyano column etc., its fill out cleanser kind relatively fixing (being generally 1 ~ 2 two kind of filler), mainly there is stronger selective adsorption to the impurity in extract, reach the object of removal, and the adsorbability of the object in extract in cleanser is lower, can not loses because of purification run.Commodity decontaminating column is better to the removal effect of some impurity as albumen, pigment, but there is following defect: 1) contain plurality of impurities in usual environmental sample, and the filling agent of decontaminating column mostly is the functional cleanser removing single contaminant, reach desirable purification object, dissimilar decontaminating column must be connected in series, add processing cost; 2) the usual compactness of the filler of commodity decontaminating column is higher, and density is large, and when the extract purified contains the macromolecular organism such as humic acid, purification rate reduces greatly, even blocks; 3) for the target organic that adsorbability is stronger, the decontaminating column of plastic material more can cause the absorption of object to remain, and causes object to lose; For some plastifier class object, plastics decontaminating column then can produce introduces external source pollution, occurs false-positive result.
In addition, existing homemade purification chromatographic column mostly is integral type, non-dismountable, after sample extracting solution purification, decontaminating column be washed to as a difficult problem, a part of reason purification pipe is longer, filling agent through dehydration, deproteinized, after the operation such as degrease, pressure comparatively real, does not have suitable utensil to be difficult to remove cleanser, only discards cleanser waste time and energy by removing from entrance point vibration or shake after being inverted, and easily cause purification pipe damaged, get half the result with twice the effort.Purification pipe Design of length is unreasonable simultaneously also easily causes effective purge volume to reduce, the disadvantages such as purification efficiency reduction; Or will ensure enough purification efficiencies, extract need be carried out pre-concentration, to reduce the use amount of cleanser, what make the operation of sample pre-treatments become is loaded down with trivial details.
Utility model content
The purpose of this utility model is to provide a kind of good airproof performance, simple to operate, reusable, the chromatography decontaminating column of being convenient to the middle volume sample extract cleaned.
For achieving the above object, the chromatography decontaminating column of middle volume sample extract of the present utility model, comprises and managing under interconnective cleanser splendid attire Guan Shangguan and cleanser splendid attire pipe from top to bottom, wherein:
The structure that described cleanser splendid attire Guan Shangguan is integrated, be followed successively by application of sample portion, dilatation portion and connecting portion from top to bottom, wherein, the internal diameter ratio of application of sample portion, dilatation portion and connecting portion is 4: (5 ~ 6): 3, length ratio is 1: (3 ~ 4): 5, the caliber in dilatation portion is obviously coarser than application of sample portion, and object is for holding the main body of extract; Be provided with glass crotch down in the upper end in dilatation portion, be mainly used in chromatography decontaminating column being affiliated in without support situation completing purification run on miscellaneous equipment or object; The lower end of connecting portion is provided with upwards curved glass crotch.The caliber of connecting portion is less than dilatation portion, and its length is greater than dilatation portion, thus can ensure the cleanser of filling q.s.
Under described cleanser splendid attire pipe, the upper end of pipe is provided with decurved glass crotch, and lower end has activity cock;
Under described cleanser splendid attire pipe, the upper end of pipe is embedded with silica sand pad, and Main Function is carrying cleanser, prevention cleanser runs off and block system;
The chromatography of socket formation mutually decontaminating column is managed under described cleanser splendid attire Guan Shangguan and cleanser splendid attire pipe.
Described chromatography decontaminating column also comprises glass stopper, and the outside of described glass stopper and the inwall of application of sample portion bottleneck are ground structure, and described glass stopper is arranged in the bottleneck in application of sample portion, can reduce the volatilization of liquid by arranging glass stopper.
Preferably, described cleanser splendid attire Guan Shangguan is connected by ground with pipe under cleanser splendid attire pipe.
In a preferred embodiment, under the glass crotch of described cleanser splendid attire Guan Shangguan lower end and cleanser splendid attire pipe, the glass crotch of pipe upper end is fastened by elastic rubber circle, by elastic rubber circle, glass crotch corresponding for pipe under cleanser splendid attire Guan Shangguan and cleanser splendid attire pipe is strained, thus fixing chromatographic column is overall.
Preferably, described silica sand pad is aperture 100 object glass sand sheet, and the diameter of described silica sand pad equals the external diameter of the ground of connecting portion lower end.
Preferably, under described cleanser splendid attire pipe, pipe is provided with the polytetrafluoro cock of intermediate throughholes, by rotating described polytetrafluoro cock, can control the purification rate of liquid in chromatography purification pipe.
Preferably, under described cleanser splendid attire Guan Shangguan and cleanser splendid attire pipe the length of pipe than being (2.5 ~ 3): 1.
Beneficial effect: compared with prior art, middle volume sample extract chromatography purification pipe tool of the present utility model has the following advantages:
(1) by purification pipe is divided into two parts, and connect with ground Nesting Technique, realize the detachable of purification pipe, be convenient to the removing of discarded cleanser;
(2) different size is become by the pipe diameter determing of each several part of purification pipe, the disposable interpolation (ensureing to hold) of volume extract in realization, the anti-short stream of efficient successively purification of extract, the object adjustable with purification flow velocity, makes whole operation reasonable, smooth;
(3) connection between device all parts adopts ground and the design of frosted mouth mostly, synchronously achieves impermeability and the detachability of device; The glass sand sheet of carrying cleanser is separate unit, both after inserting, effectively can carry cleanser, and can remove cleanser fast afterwards again in taking-up;
(4) for the purification of middle volume sample (30 ~ 70ml) extract, pre-concentration one step can be exempted; And according to the preanalysis of extract impurity, the composite purifying agent filler of more than 3 kinds can be added targetedly, realize the high efficiency of purification.
Accompanying drawing explanation
Fig. 1 is structural representation of the present utility model.
Embodiment
Below in conjunction with structural representation, the utility model is further described.
As shown in Figure 1, the utility model provides volume sample extract chromatography decontaminating column in one, comprises cleanser splendid attire Guan Shangguan 1, pipe 2 under cleanser splendid attire pipe, cleanser carrying silica sand pad 3, connection elastic rubber circle 4.Cleanser splendid attire Guan Shangguan 1 is integral type structure, and it comprises three parts, is respectively application of sample portion 5, dilatation portion 6 and connecting portion 7, wherein, application of sample portion 5 is namely as the bottleneck of chromatography decontaminating column, and in the present embodiment, the length of bottleneck is 3cm, internal diameter is 2.4cm, wall thickness 2.5mm, bottleneck designs for ground, and the inside is provided with glass stopper 8, the outside of glass stopper 8 and the inwall of application of sample portion 5 bottleneck are ground structure, and glass stopper 8 is arranged in the bottleneck in application of sample portion.The caliber in dilatation portion 6 is 2.9cm, length is 10cm, it, as holding the main body of extract, is provided with glass crotch 9 down in the upper end in dilatation portion, be mainly used in being affiliated to by chromatography decontaminating column in without support situation completing purification run on miscellaneous equipment or object.The caliber of connecting portion 7 is 1.8cm, length is 15.5cm, and its lower end is designed, for being connected by ground with pipe 2 under cleanser splendid attire pipe for ground, the lower end of connecting portion is provided with upwards curved glass crotch, and under cleanser splendid attire pipe, the upper end of pipe 2 is provided with upwards curved glass crotch.Under cleanser splendid attire pipe, the length of pipe 2 is 10cm.
The cleanser carrying upper end of pipe 2 under silica sand pad 3 activity embedding cleanser splendid attire pipe, under cleanser splendid attire Guan Shangguan 1 and cleanser splendid attire pipe, pipe 2 is by ground nested encryptions, airtight, then with elastic rubber circle 4, cleanser splendid attire Guan Shangguan 1 is connected with the glass crotch of pipe 2 under cleanser splendid attire pipe, be an entirety, under cleanser splendid attire pipe, pipe 2 has the activity cock 10 of polytetrafluoro material simultaneously, can control the speed of extract purification.
The use procedure of the chromatography decontaminating column of middle volume sample extract of the present utility model is divided into four parts:
(1) assemble.Cleanser is carried silica sand pad is smooth to be put under cleanser splendid attire pipe after pipe, managing cleanser splendid attire Guan Shangguan under ground end inserts cleanser splendid attire pipe, screws ground by the power of appropriateness, to ensure sealing.Elastic rubber snare is lived the glass crotch of pipe under corresponding cleanser splendid attire Guan Shangguan and cleanser splendid attire pipe, make decontaminating column become to be integrated, the polytetrafluoro cock of pipe under cleanser splendid attire pipe is inserted, screws piston, with liquid-leakage preventing.
(2) post is filled, according to the volume of extract, by appropriate dissimilar cleanser subsection filling in chromatography decontaminating column, the solvent identical with extract composition is added from the upper end of chromatography decontaminating column, rinse and activation (simultaneously reducing the loss that solvent absorption causes) are carried out to cleanser, after solvent-soaked cleanser, to outward winding the polytetrafluoro cock of lower end, rinse liquid is dropwise flowed out, when chromatography decontaminating column solvent liquid level is about to lower than cleanser top, close the polytetrafluoro cock of lower end, cover decontaminating column with ground glass stopper simultaneously, prevent solvent from volatilizing;
(3) purify, open top seal plug, middle volume sample extract is all poured into, regulate the cock of decontaminating column lower end, control purification rate at 1 drop/sec, make whole extract flow through decontaminating column, complete purification run, after liquid to be extracted all purifies, then cross decontaminating column with a small amount of solvent, object residual on cleanser may be adsorbed on to wash out.
(4) purging system, open the elastic rubber circle for connecting, outward winding cleanser splendid attire Guan Shangguan with pipe ground coupling part under cleanser splendid attire pipe, take out glass yarn sheet, shake cleanser splendid attire Guan Shangguan gently, abandon taking out with the cleanser crossed, the polytetrafluoro cock of pipe under cleanser splendid attire pipe is removed, each assembly of the chromatography decontaminating column of volume sample extract in cleaning, completes the chromatography purification run of sample extracting solution.
Introduce the using method of the utility model device below for the purification of the atrazine extract in Cipangopaludina chinensis sample, concrete flow process comprises the steps:
(1) assembling of decontaminating column: cleanser is carried silica sand pad is smooth to be put under cleanser splendid attire pipe after pipe, manages cleanser splendid attire Guan Shangguan, screws ground by the power of appropriateness, to ensure sealing under ground end inserts cleanser splendid attire pipe.Elastic rubber snare is lived the glass crotch of pipe under corresponding cleanser splendid attire Guan Shangguan and cleanser splendid attire pipe, make decontaminating column become to be integrated, the polytetrafluoro cock of pipe under cleanser splendid attire pipe is inserted, screws piston, with liquid-leakage preventing.
(2) selection of cleanser: in Cipangopaludina chinensis, the extraction of atrazine mainly adopts acetonitrile and ethyl acetate mixed solvent to carry out, the volume of extract is 30 ~ 50mL, the main interference impurity that may exist in extract is moisture, protein and grease, for this three classes impurity, the cleanser selected is respectively anhydrous sodium sulfate, anhydrous zinc sulfate and neutral alumina.
(3) filling of cleanser: with reference to the composition of existing data about this few class impurity in this bio-matrix, the mass ratio according to 2: 3: 3 fills anhydrous zinc sulfate, anhydrous sodium sulfate and neutral alumina.
(4) activation of cleanser: pipette the acetonitrile of 10ml ~ 20ml in decontaminating column, rinse, activating and purifying agent, the aperture of cock bottom adjustment decontaminating column, makes scavenging solution dropwise flow out, when solvent interface is about to lower than cleanser top, move into the ethyl acetate of 10ml ~ 20ml again, the aperture of cock bottom adjustment decontaminating column, makes scavenging solution dropwise flow out, when solvent interface is about to lower than cleanser top, cut-out tap, covers the end suitable for reading of decontaminating column with ground glass stopper.
(5) purification of extract: open top glass plug, all pours decontaminating column into by disposable for the extract of spiral shell, and the cock of adjustment decontaminating column lower end, makes the speed that oozes of scavenging solution maintain 3ml/min, collection and purification liquid.Liquid to be extracted all by after decontaminating column, then with extract remaining in the acetonitrile ethyl acetate mixed solvent wash-out post of 1: 1 of 5ml, completes purification run.

Claims (7)

1. a chromatography decontaminating column for volume sample extract in, comprises and managing under interconnective cleanser splendid attire Guan Shangguan and cleanser splendid attire pipe from top to bottom, it is characterized in that:
Described cleanser splendid attire Guan Shangguan is followed successively by application of sample portion, dilatation portion and connecting portion from top to bottom, wherein, the internal diameter ratio of application of sample portion, dilatation portion and connecting portion is 4: 5 ~ 6: 3, length ratio is 1: 3 ~ 4: 5, be provided with glass crotch down in the upper end in dilatation portion, the lower end of connecting portion is provided with upwards curved glass crotch;
Under described cleanser splendid attire pipe, the upper end of pipe is provided with decurved glass crotch, and lower end has activity cock;
Under described cleanser splendid attire pipe, the upper end of pipe is embedded with silica sand pad;
The chromatography of socket formation mutually decontaminating column is managed under described cleanser splendid attire Guan Shangguan and cleanser splendid attire pipe.
2. chromatography decontaminating column according to claim 1, is characterized in that, described chromatography decontaminating column also comprises glass stopper, and the outside of described glass stopper and the inwall of application of sample portion bottleneck are ground structure, and described glass stopper is arranged in the bottleneck in application of sample portion.
3. chromatography decontaminating column according to claim 1, is characterized in that, described cleanser splendid attire Guan Shangguan is connected by ground with pipe under cleanser splendid attire pipe.
4. chromatography decontaminating column according to claim 1, is characterized in that, under the glass crotch of described cleanser splendid attire Guan Shangguan lower end and cleanser splendid attire pipe, the glass crotch of pipe upper end is fastened by elastic rubber circle.
5. chromatography decontaminating column according to claim 1, is characterized in that, described silica sand pad is aperture 100 object glass sand sheet, and the diameter of described silica sand pad equals the external diameter of the ground of connecting portion lower end.
6. chromatography decontaminating column according to claim 1, is characterized in that, under described cleanser splendid attire pipe, pipe is provided with the polytetrafluoro cock of intermediate throughholes.
7. chromatography decontaminating column according to claim 1, is characterized in that, under described cleanser splendid attire Guan Shangguan and cleanser splendid attire pipe, the length ratio of pipe is 2.5 ~ 3: 1.
CN201520682243.8U 2015-09-06 2015-09-06 Chromatography purifying column of well volume sample extract Expired - Fee Related CN204924760U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201520682243.8U CN204924760U (en) 2015-09-06 2015-09-06 Chromatography purifying column of well volume sample extract

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Application Number Priority Date Filing Date Title
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106525547A (en) * 2016-11-21 2017-03-22 百奥森(江苏)食品安全科技有限公司 Chromatography purifying column for medium-volume sample extract

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106525547A (en) * 2016-11-21 2017-03-22 百奥森(江苏)食品安全科技有限公司 Chromatography purifying column for medium-volume sample extract

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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: 20151230

Termination date: 20180906

CF01 Termination of patent right due to non-payment of annual fee