CN102350327A - Novel hydrophilic C18 filling material and its solid phase extraction column - Google Patents
Novel hydrophilic C18 filling material and its solid phase extraction column Download PDFInfo
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- CN102350327A CN102350327A CN201110231016XA CN201110231016A CN102350327A CN 102350327 A CN102350327 A CN 102350327A CN 201110231016X A CN201110231016X A CN 201110231016XA CN 201110231016 A CN201110231016 A CN 201110231016A CN 102350327 A CN102350327 A CN 102350327A
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Abstract
The invention relates to a resin surface modified novel material and a solid phase extraction column, which relates to the chemical technical field. The solid phase extracting resin surface modified novel material has the difference of the mean particle diameter in a range of between -20 and 20 percent, the difference of the specific weight is in a range of between -20 and 20 percent. The solid phase extraction mixed filling material is used for preparing the solid phase column, the mixed filling material is filled in the column tube, sieve plates are provided outside of two ends of the filling material for preventing the mixed filling material from leaking, one end of the column tube is for loading and the other end of the column tube is for flowing out, an eluent enters into the solid phase extraction column from a loading aperture. The characteristic application of the present invention is a selective extraction of a polar and nonpolar compound in a solution under water environment.
Description
Technical field
The present invention relates to technical field of analytical chemistry, the new material and the solid-phase extraction column thereof of two kinds of functional groups of particularly a kind of silica gel surface bond.
Background technology
Novel hydrophilic C18 material is a kind of widely used sample pre-treatments technology filler; The sample pre-treatments technology for the SPE basic principle be in the sample with fixing have mutually pretend component firmly and on solid-phase extraction column, keep; And flow out solid-phase extraction column very soon, thereby reach the separation purpose with the more weak component of fixing active force mutually.
Use more SPE material to mainly contain bonded silica gel SPE material, inorganic matrix SPE material, organic polymer SPE material and mixed type SPE material 4 big classes at present.
Wherein using maximum is carbon 18 bonded silica gel solid-phase extraction columns; Generally regarded universal adsorbent; Can be from the aqueous solution adsorb organic compound; Especially be suitable for organic desalination, its major defect be selectivity low, to strong polarity and water-soluble sample keep weak, volume containing the sample is low, dust removal rate is low etc.
The inorganic matrix solid material mainly is inorganic oxide and graphitized carbon class inorganic matter, and the common feature of these inorganic material is that the surface has activity hydroxy, is mainly used in the positive extraction.
Organic polymer SPE material is that matrix is carried out surface modified with SDEB styrene diethylenebenzene copolymer resins (PS); In recent years; Constantly there is new high-crosslinking-degree polymer resin SPE material to put on market, as contains methylol, benzoyl and adjacent carboxylbenzoyl, sulfonic group, quaternary ammonium salt etc.These modified resin have good hydrophily, when extraction water Semi-polarity compound, can obtain the higher rate of recovery.
Mixed type SPE material mainly is that solid-phase extraction column is inserted in sorbing material layering more than 2 kinds or 2 kinds; Reach under the prerequisite of not losing target compound; Utilize the characteristic of mixed type solid-phase extraction column different functional groups, remove the purpose of sample substrate intermediate ion type and nonpolar chaff interference through the pH value in the adjusting extraction process respectively.
But above material all has its defective, and especially silica gel material is for the rate of recovery poor effect of strong water-soluble sample, and the binding ability that therefore is necessary to develop a kind of C18 filler and water is stronger, can from water, extract the strong water-soluble sample, the enhancing gas recovery rate.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, be provided at the new material of two kinds of functional groups of same silica gel finishing.
The technical scheme that the present invention adopts is following:
Two kinds of functional groups are bonded to the silica matrix surface through chemical method, two kinds of functional groups are bonded in the silica gel surface simultaneously, thereby on a kind of material, bring into play two kinds of functional group's advantages, thereby better realize the purpose of SPE.
1, novel hydrophilic C18 new material and solid-phase extraction column thereof is characterized in that: through in two kinds of different functional groups of silica gel material surface bond, obtain polymer overmold type silica gel absorption new material.
This resin-coated silica gel new material can be made into solid-phase extraction column.
2, silica gel surface modification new material according to claim 1; It is characterized in that: be included in two kinds of groups of silica gel surface bond octadecyl and methyl; Through hybrid bonded mode of a step; Control different functional groups ratio is 100: 1-1: 100; Average grain diameter differ+/-20% in, proportion differ+/-20% in;
3, be octadecyl trim,ethylchlorosilane and MTMS according to the said described silica gel surface modification new material of claim 2.
4, the solid-phase extraction column processed of the described hydrophilic C18 silica gel new packing of claim 1; It is characterized in that: column jecket inside is carried and is filled new type resin coating silica filler; The filler two ends are sealed by sieve plate; Prevent that mixed fillers from leaking outside; Column jecket one end is sample or solvent inlet; One end is sample or solvent streams outlet, and sample or solvent inject from pillar one end.
5, solid-phase extraction column according to claim 4 is characterized in that: column jecket is a polypropylene plastics, and its volume is the 0.1-100 milliliter.
6, solid-phase extraction column post according to claim 5 is characterized in that: contain 0-100% water in the described flowing phase, Applicable temperature is 5-50 ℃.
The beneficial effect that the present invention had:
1, the present invention can be soaked into 100% fully, according to the wider scope of application is arranged;
2, the present invention all has the good adsorption effect to organic compound, has wider range of application;
3, selectivity of the present invention is good, highly versatile, and volume containing the sample is high;
4, filler synthesis step of the present invention is simple, easy production in batch, good reproducibility.
Description of drawings
Fig. 1 is the solid-phase extraction column sketch map;
Among the figure, 1-1 is the medical grade polypropylene pipe, and 1-2 is sieve plate (the porous polypropylene materials of 20 μ m), and 1-3 is a filler, and 1-4 is a general-purpose interface.
The specific embodiment
Below in conjunction with specific embodiment the present invention is described further.
Embodiment 1:
The preparation of two kinds of functional group's bonded silica gel new materials
10000ml 5000ml four-necked flask was added toluene 1.5kg diameter of
silica gel, dehydrated to a dry state (1min under water drops date), then cooled to 80 ℃, add pre-mixed silane (octadecyl trichlorosilane: A trimethoxysilane = 8:2; Note: mixing ratio of the mass ratio) 600g, and imidazole 400g, heated to 120 ℃, and 120 ± 1 ℃ incubated for 12 hours, cooling the material.
Above-mentioned filler is dried with centrifuge; With 4500ml toluene wash 3 times; With 4500ml methanol wash 3 times; The mixed solution that adds 300ml water with the 4000ml oxolane soaked 1 hour; Then with 4500m oxolane washing 3 times; With 4500ml methanol wash 3 times, then 100 ℃ of vacuum drying 10 hours finished product.
Embodiment 2:
The preparation of two kinds of functional group's silica gel new material substep bondings
First step: 10000ml 5000ml four-necked flask was added toluene, 1.5kg diameter of
silica gel, dehydrated to anhydrous state (1min under water drops prevail), and then cooled to 80 ℃, adding octadecyltrimethylammonium chlorosilane 500g, and imidazole 300g, heated to 120 ℃, and 120 ± 1 ℃ incubated for 12 hours, cooling the material.
Above-mentioned filler is dried with centrifuge; With 4500ml toluene wash 3 times; With 4500ml methanol wash 3 times; The mixed solution that adds 300ml water with the 4000ml oxolane soaked 1 hour; Then with 4500m oxolane washing 3 times; With 4500ml methanol wash 3 times, then 100 ℃ of vacuum drying 10 hours semi-finished product.
Second step: the toluene and the above-mentioned reaction gained semi-finished product that in the 10000ml four-hole boiling flask, add 5000ml; Dewater to anhydrous state (1min do not have water droplet drip be as the criterion); Be cooled to 80 ℃ then; Add MTMS 500g; Add imidazoles 300g then; Be warming up to 120 ℃, and 120 ± 1 ℃ are incubated 12 hours, cooling discharging.
Above-mentioned filler is dried with centrifuge; With 4500ml toluene wash 3 times; With 4500ml methanol wash 3 times; The mixed solution that adds 300ml water with the 4000ml oxolane soaked 1 hour; Then with 4500m oxolane washing 3 times; With 4500ml methanol wash 3 times, then 100 ℃ of vacuum drying 10 hours finished product.
Embodiment 3:
The surface modified new material of silica gel is taken by weighing 500mg, pack band into down in the 6ml column jecket of sieve plate, insert behind the upper sieve plate evenly, use the presser-into-rod compacting with the concussion of vibrations bed.
Embodiment 4:
Pillar is 3 earlier in the instance 3, and respectively with 5ml methyl alcohol, 0.5mol/L H is used in the activation of 5ml water
2SO
4Regulate pH to 1.5～2 of 300mL water sample, flow through pillar, 5mL water wash pillar with the flow velocity of 4～5mL/min; Blow pillar 20min with nitrogen, then with the residual moisture in the 0.9mL methyl alcohol displacement pillar, then with 5mL oxolane wash-out; Nitrogen is concentrated into 1mL, analyzes with HPLC.
Embodiment 5:
Pillar is 3 earlier in the instance 3, and respectively with 5ml methyl alcohol, isopropyl alcohol concentration to 10% is added in the activation of 5ml water in the 300mL water sample, flows through pillar with the flow velocity of 4～5mL/min.Owing to polycyclic aromatic hydrocarbon can be lost by the absorption of container and pipeline,, go up then kind to post so deposit the container bottle and the transfer pipeline of water sample with 50% the isopropanol water solution rinse of 10mL.5mL water wash pillar.Blow pillar 20min with nitrogen, with the residual moisture in the 0.9mL methyl alcohol displacement pillar, then use 5mL methyl alcohol: carrene (3: 7) mixed liquor wash-out then; Nitrogen is concentrated into 1mL, analyzes with HPLC.
The above only is preferred embodiment of the present invention, is not technical scheme of the present invention is done any pro forma restriction.Every foundation technical spirit of the present invention all still belongs in the scope of technical scheme of the present invention any simple modification, equivalent variations and modification that above embodiment did.
Claims (6)
1. novel hydrophilic C18 new material and solid-phase extraction column thereof is characterized in that: through in two kinds of different functional groups of silica gel material surface bond, obtain polymer overmold type silica gel absorption new material.
This polymer overmold silica gel new material can be made into solid-phase extraction column.
2. silica gel surface modification new material according to claim 1; It is characterized in that: be included in two kinds of groups of silica gel surface bond octadecyl and methyl; Through hybrid bonded mode of a step; Control different functional groups ratio is 100: 1-1: 100; Average grain diameter differ+/-20% in, proportion differ+/-20% in.
3. silica gel surface modification new material according to claim 2 is octadecyl trim,ethylchlorosilane and MTMS.
4. the solid-phase extraction column that hydrophilic C18 silica gel new packing according to claim 1 is processed; It is characterized in that: column jecket inside is carried and is filled new type resin coating silica filler; The filler two ends are sealed by sieve plate; Prevent that mixed fillers from leaking outside; Column jecket one end is sample or solvent inlet; One end is sample or solvent streams outlet, and sample or solvent inject from pillar one end.
5. solid-phase extraction column according to claim 4 is characterized in that: column jecket is a polypropylene plastics, and its volume is the 0.1-100 milliliter.
6. solid-phase extraction column according to claim 5 is characterized in that: contain 0-100% water in the described flowing phase, Applicable temperature is 5-50 ℃.
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| CN201110231016XA CN102350327A (en) | 2011-08-12 | 2011-08-12 | Novel hydrophilic C18 filling material and its solid phase extraction column |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103877747A (en) * | 2012-12-21 | 2014-06-25 | 上海磐合科学仪器股份有限公司 | Solid-phase extraction column |
| CN105413666A (en) * | 2015-11-24 | 2016-03-23 | 徐州医学院 | Solid-phase extraction filler, solid-phase extraction column and preparation method and application of solid-phase extraction filler |
| CN105817053A (en) * | 2015-08-05 | 2016-08-03 | 台湾多胺股份有限公司 | Extraction apparatus, extraction system and extraction method for physiological active substances in urine |
| CN106289895A (en) * | 2015-06-05 | 2017-01-04 | 吉林出入境检验检疫局检验检疫技术中心 | A kind of ecological textile venomous injurant quality detection decontaminating column and preparation method thereof |
| CN108051279A (en) * | 2017-06-26 | 2018-05-18 | 青岛贞正分析仪器有限公司 | It is a kind of for pre-treatment decontaminating column of Mycotoxin identification and preparation method thereof |
| CN109589950A (en) * | 2019-01-11 | 2019-04-09 | 上海谱宁分析技术有限公司 | A kind of preparation method of liquid chromatographic packing materials |
| CN111228855A (en) * | 2020-01-14 | 2020-06-05 | 无锡市疾病预防控制中心 | Preparation method of pineapple pulp matrix biochar filler solid-phase extraction column |
| CN117019122A (en) * | 2023-09-25 | 2023-11-10 | 苏州宇莘新材料有限公司 | Preparation method of novel hydrophilic alkyl bonded silica gel filler |
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| US5279742A (en) * | 1991-02-07 | 1994-01-18 | Minnesota Mining And Manufacturing Company | Solid phase extraction medium |
| CN1704140A (en) * | 2004-05-28 | 2005-12-07 | 北京大学 | Filling material used for molecule brand solid phase extraction and preparation method thereof |
| CN101628223A (en) * | 2008-07-18 | 2010-01-20 | 华东理工大学 | Monolithic silica gel adsorption column, and solid phase extraction device and application thereof |
| CN101721980A (en) * | 2009-11-13 | 2010-06-09 | 天津博纳艾杰尔科技有限公司 | Mixed fillers of liquid-phase chromatographic column and chromatographic column |
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| US5279742A (en) * | 1991-02-07 | 1994-01-18 | Minnesota Mining And Manufacturing Company | Solid phase extraction medium |
| CN1704140A (en) * | 2004-05-28 | 2005-12-07 | 北京大学 | Filling material used for molecule brand solid phase extraction and preparation method thereof |
| CN101628223A (en) * | 2008-07-18 | 2010-01-20 | 华东理工大学 | Monolithic silica gel adsorption column, and solid phase extraction device and application thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103877747A (en) * | 2012-12-21 | 2014-06-25 | 上海磐合科学仪器股份有限公司 | Solid-phase extraction column |
| CN106289895A (en) * | 2015-06-05 | 2017-01-04 | 吉林出入境检验检疫局检验检疫技术中心 | A kind of ecological textile venomous injurant quality detection decontaminating column and preparation method thereof |
| CN106289895B (en) * | 2015-06-05 | 2019-05-07 | 吉林出入境检验检疫局检验检疫技术中心 | A kind of ecological textile venomous injurant quality detection decontaminating column and preparation method thereof |
| CN105817053A (en) * | 2015-08-05 | 2016-08-03 | 台湾多胺股份有限公司 | Extraction apparatus, extraction system and extraction method for physiological active substances in urine |
| CN105817053B (en) * | 2015-08-05 | 2018-01-30 | 台湾多胺股份有限公司 | Extraction equipment, extracting system and the method for extracting urine physiological activator of urine physiological activator |
| CN105413666A (en) * | 2015-11-24 | 2016-03-23 | 徐州医学院 | Solid-phase extraction filler, solid-phase extraction column and preparation method and application of solid-phase extraction filler |
| CN105413666B (en) * | 2015-11-24 | 2017-10-24 | 徐州医学院 | A kind of solid phase extraction filler, solid phase extraction column and its preparation method and application |
| CN108051279A (en) * | 2017-06-26 | 2018-05-18 | 青岛贞正分析仪器有限公司 | It is a kind of for pre-treatment decontaminating column of Mycotoxin identification and preparation method thereof |
| CN109589950A (en) * | 2019-01-11 | 2019-04-09 | 上海谱宁分析技术有限公司 | A kind of preparation method of liquid chromatographic packing materials |
| CN111228855A (en) * | 2020-01-14 | 2020-06-05 | 无锡市疾病预防控制中心 | Preparation method of pineapple pulp matrix biochar filler solid-phase extraction column |
| CN117019122A (en) * | 2023-09-25 | 2023-11-10 | 苏州宇莘新材料有限公司 | Preparation method of novel hydrophilic alkyl bonded silica gel filler |
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Application publication date: 20120215 |