CN1772329A - Extracting head for solid phase micro extraction of dextrin derivative and its making process - Google Patents
Extracting head for solid phase micro extraction of dextrin derivative and its making process Download PDFInfo
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- CN1772329A CN1772329A CN 200510019797 CN200510019797A CN1772329A CN 1772329 A CN1772329 A CN 1772329A CN 200510019797 CN200510019797 CN 200510019797 CN 200510019797 A CN200510019797 A CN 200510019797A CN 1772329 A CN1772329 A CN 1772329A
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Abstract
The extracting head for solid phase micro extraction of cyclodextrin derivative includes quartz fiber and its coating and the coating is composite coating of 2, 6-di-oxy-methyl-beta-cyclodextrin and hydroxyl silicon oil bonded to the surface of the quartz fiber. The preparation process of the extracting head includes the following steps: diluting 2, 6-di-oxy-methyl-beta-cyclodextrin with dichloromethane, adding hydroxyl silicon oil, tetraethoxy silane, 3-(2, 3-epoxy propane) propyl trimethoxy silane and water containing trifluoro acetic acid, adding hydrogen-containing silicon oil, ultrasonic vibration and centrifuging, and taking supernatant; inserting one end of the quartz fiber after eliminating protecting layer and drying into the sol liquid, taking out, drying and ageing under the protection of nitrogen to obtain the extracting head. The present invention has high heat stability, high solvent flush resistance, long service life, high in Benzedrine medicine capacity and excellent application foreground in medicine analysis, including stimulant detection.
Description
Technical field
The present invention relates to a kind of extracting head for solid phase micro extraction of dextrin derivative and preparation method thereof, promptly 2, composite coating solid phase micro-extraction extraction head of 6-two-O-methyl-beta-schardinger dextrin-and hydroxy silicon oil and preparation method thereof belongs to chemical field, also belongs to the analytical chemistry field.
Background technology
SPME is a kind of centralized procurement sample, concentrate, sample introduction is in one, sensitive, solvent-free sample-pretreating method simply, fast,, its initial fields such as environment, food, aroma analysis that concentrate on of using, it is got more and more and is applied to medical sample analysis in recent years.In the complex biological matrix drug sample analysis (for example, the detection of stimulants in the human body fluid) of trace, trace to the proposition of the selectivity of SPME and sensitivity requirements at the higher level.And the extracting head coating kind of commercial SPME is limited, be difficult to satisfy the demand, and most commercial extracting head adopts physics to be coated with stain and partial cross-linked method preparation, is difficult to avoid operating temperature low, and anti-solvent washing ability such as is lacked service life at weakness.Therefore, use that new coating material prepares that selectivity is good, extraction efficiency is high, the new coating of good operation performance, long service life becomes the research focus of solid phase micro-extraction technique.
Summary of the invention
The object of the present invention is to provide a kind of extracting head for solid phase micro extraction of dextrin derivative and preparation method thereof, promptly with 2,6-two-O-methyl-beta-schardinger dextrin-and hydroxy silicon oil are coating material, adopt sol-gel process to prepare solid phase micro-extraction extraction head.This extracting head should have heat endurance and solvent stability is good, and long service life has characteristics such as fine extracting power to the amphetamine stimulant substance.
For achieving the above object, the technical solution adopted in the present invention is as follows:
A kind of extracting head for solid phase micro extraction of dextrin derivative comprises that quartz fibre reaches the coating attached to the quartz fibre surface, and described coating is to be bonded in 2 of quartz fibre surface, 6-two-O-methyl-beta-schardinger dextrin-and hydroxy silicon oil composite bed.
The present invention also provides the preparation method of above-mentioned solid phase micro-extraction extraction head: get 20-60mg2,6-two-O-methyl-beta-schardinger dextrin-, dilute with 100-250 μ L carrene, add the 80-120mg hydroxy silicon oil, add 90-150 μ L tetraethoxysilane (or MTMS), add 30-70 μ L3-(2, the 3-expoxy propane) propyl trimethoxy silicane, the trifluoroacetic acid that adds the 60-100 moisture 3%-8% of μ L (volume ratio), the containing hydrogen silicone oil that adds 2-15mg then, sonic oscillation 3-10 minute, under 8000-16000r/min centrifugal 5-8 minute, it was standby to take out supernatant liquor.Quartz fibre one end that removes the drying of protective layer is inserted about 30-60min in the colloidal sol clear liquid, and repeatable operation obtains certain thickness coating for several times, takes out the back and places 12-24 hour in drier, at N
2Protection promptly gets required solid phase micro-extraction extraction head in 250-320 ℃ of aging 2-3h down.
Description of drawings
Fig. 1 is the influence of high temperature to the probe extraction quantity;
Fig. 2 is the influence of solvent to the probe extraction quantity;
Fig. 3 is the influences of access times to the probe extraction quantity;
Fig. 4 is that the extracting power of extracting head and commercial PDM S and PA probe compares.
The specific embodiment
Below in conjunction with specific embodiment technical scheme of the present invention is further described:
In the embodiment of the invention, 2,6-two-O-methyl-beta-schardinger dextrin-is synthetic by this laboratory reference literature method (J.-M.Lehn, Helv.Chim.Acta.61 (1978) 2190 for R.J.Boger, R.J.Corcoran).Hydroxy silicon oil (OH-TSO, molecular weight are 3000-5000) is used and the research center available from Chengdu silicon, tetraethoxysilane, MTMS, 3-(2, the 3-expoxy propane) propyl trimethoxy silicane, containing hydrogen silicone oil (molecular weight is 1000-3000) is available from the Wuhan University chemical plant.Trifluoroacetic acid is available from the Beijing Chemical Plant.
Embodiment 1:
Get 30mg2,6-two-O-methyl-beta-schardinger dextrin-with the dilution of 150 μ L carrene, adds 90mg hydroxy silicon oil (molecular weight is 4000), add 100 μ L tetraethoxysilanes (or MTMS), add 50 μ L3-(2, the 3-expoxy propane) propyl trimethoxy silicane, add the trifluoroacetic acid of 75 μ L moisture 8% (volume ratio), the containing hydrogen silicone oil (molecular weight is 2000) that adds 5mg then, sonic oscillation 5 minutes, under 8000r/min centrifugal 8 minutes, it was standby to take out supernatant liquor.Quartz fibre one end that removes the drying of protective layer is inserted about 40min in the colloidal sol clear liquid, and repeatable operation obtains certain thickness coating for several times, takes out the back and places 18 hours in drier, at N
2Protection promptly gets required solid phase micro-extraction extraction head in 300 ℃ of aging 2h down.
Embodiment 2:
Get 60mg2,6-two-O-methyl-beta-schardinger dextrin-, dilute with 220 μ L carrene, add 100mg hydroxy silicon oil (molecular weight is 5000), add 150 μ L tetraethoxysilanes (or MTMS), add 60 μ L3-(2, the 3-expoxy propane) propyl trimethoxy silicane, the trifluoroacetic acid that adds 100 μ L moisture 5% (volume ratio), the containing hydrogen silicone oil that adds 10mg (molecular weight is 3000) then, sonic oscillation 8 minutes, under 16000r/min centrifugal 5 minutes, it was standby to take out supernatant liquor.Quartz fibre one end that removes the drying of protective layer is inserted about 60min in the colloidal sol clear liquid, and repeatable operation obtains certain thickness coating for several times, takes out the back and places 24 hours in drier, at N
2Protection promptly gets required solid phase micro-extraction extraction head in 250 ℃ of aging 3h down.
Adopt the obtained beneficial effect of technical scheme of the present invention:
The present invention adopts sol-gel technology preparing 2,6-two-O-methyl-beta-schardinger dextrin-/hydroxy silicon oil (solid phase micro-extraction extraction head of DM-β-CD/OH-TSO).This technical scheme relates to the hydrolysis of two kinds of monomers, and a kind of is the three-dimensional silica gel skeleton that the tetraethoxysilane hydrolysis forms an inorganic medium; Another kind is silane coupler 3-(2, a 3-expoxy propane) propyl trimethoxy silicane by open loop and hydrolysis with 2, and 6-two-O-methyl-beta-schardinger dextrin-is introduced the silica gel skeleton and formed an organic whole.This organism forms firm chemical bond with the hydroxyl of glass surface again.Measure also relatively 2,6-two-O-methyl-beta-schardinger dextrin-, two kinds of compounds of hydroxy silicon oil and use CH
2Cl
2With washed 2, the infrared spectrum of 6-two-O-methyl-beta-schardinger dextrin-/hydroxy silicon oil extracting head coating, it is non-existent 2 to find to have occurred in the spectrogram of extracting head coating hydroxy silicon oil spectrogram institute, characteristic peak---the 1458.59cm of 6-two-O-methyl-beta-schardinger dextrin-
-1( OCH HCH), 1367.35cm
-1( OCH CCH) and 567.35cm
-1(ring vibration).Illustrate 2,6-two-O-methyl-beta-schardinger dextrin-successfully is bonded in the coating.
Adopt 2 of technical scheme preparation of the present invention, 6-two-O-methyl-beta-schardinger dextrin-/hydroxy silicon oil extracting head, because sol-gel technique can make the strong chemical bonding effect of generation between coating and fiber surface and the coating material, therefore has good heat endurance, anti-solvent washing ability and long service life.With two kinds of typical amphetamine stimulant substances---ephedrine (EP) and crystal methamphetamine (MA) they are test sample, examine or check the performance of this extraction probe.Fig. 1 shows 2, and 6-two-O-methyl-beta-schardinger dextrin-/hydroxy silicon oil extracting head is through 300 ℃, and the high temperature ageing of 320 ℃ and 340 ℃ is after 1 hour, and its extracting power does not descend.Fig. 2 shows 2, and 6-two-O-methyl-beta-schardinger dextrin-/hydroxy silicon oil extracting head is through CH
2Cl
2Soak respectively with water that its extraction quantity does not reduce after 10 hours, raise to some extent on the contrary, it is strong to illustrate that this extracting head anti-impact is washed ability.Can be solved by the advantage of performance sol-gel technique because high temperature, these two of solvent corrosions influence the subject matter in extracting head life-span, so the life-span of extracting head is prolonged greatly.Fig. 3 is this extracting head through the variation of extraction efficiency after 150 times the use altogether, as can be seen from the figure, and the sign that its extraction efficiency does not obviously reduce.
The cyclodextrin material has the truncated cone cavity structure of high electron density, energy and multiple compound form inclusion compound, special because its cavity size for the overwhelming majority clinical use and test in drug molecule suitable, therefore the amphetamines of being tested has been demonstrated fabulous selectivity and effect of extracting.Fig. 4 is 2,6-two-O-methyl-beta-schardinger dextrin-/hydroxy silicon oil extraction probe and two kinds of commercial probe PDMS and PA under identical extraction conditions to the comparison of the extraction efficiency of human urine epheday intermedia alkali and these two kinds of typical amphetamines of meth, as seen from the figure, the extracting power of self-control extracting head obviously is better than two kinds of commercial extracting head.
Therefore, the solid phase micro-extraction extraction head Heat stability is good of method provided by the present invention preparation, anti-solvent washing ability is strong, and long service life has good extracting power to amphetamines, comprises better application prospect being arranged aspect the drug-testing in Pharmaceutical Analysis.
Claims (2)
1. an extracting head for solid phase micro extraction of dextrin derivative comprises that quartz fibre reaches the coating attached to the quartz fibre surface, and it is characterized in that: described coating is to be bonded in 2 of quartz fibre surface, 6-two-O-methyl-beta-schardinger dextrin-and hydroxy silicon oil composite bed.
2. the preparation method of the described extracting head for solid phase micro extraction of dextrin derivative of claim 1, it is characterized in that: get 20-60mg2,6-two-O-methyl-beta-schardinger dextrin-, dilute with 100-250 μ L carrene, add the 80-120mg hydroxy silicon oil, add 90-150 μ L tetraethoxysilane or MTMS, add 30-70 μ L3-(2, the 3-expoxy propane) propyl trimethoxy silicane, the trifluoroacetic acid that adds the 60-100 moisture 3%-8% of μ L (volume ratio) adds the containing hydrogen silicone oil of 2-15mg, sonic oscillation 3-10 minute then, under 8000-16000r/min centrifugal 5-8 minute, it was standby to take out supernatant liquor; Quartz fibre one end that removes the drying of protective layer is inserted 30-60min in the colloidal sol clear liquid, take out the back and in drier, placed 12-24 hour, at N
2Protection promptly gets required solid phase micro-extraction extraction head in 250-320 ℃ of aging 2-3h down.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100197970A CN100350995C (en) | 2005-11-14 | 2005-11-14 | Extracting head for solid phase micro extraction of dextrin derivative and its making process |
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| CNB2005100197970A CN100350995C (en) | 2005-11-14 | 2005-11-14 | Extracting head for solid phase micro extraction of dextrin derivative and its making process |
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| CN100350995C CN100350995C (en) | 2007-11-28 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101972637A (en) * | 2010-09-29 | 2011-02-16 | 上海交通大学 | Triazines herbicide solid phase extraction tube and manufacturing method thereof |
| CN101992066A (en) * | 2010-09-02 | 2011-03-30 | 天津春发食品配料有限公司 | Beta-cyclodextrin substrate absorption material using glass microspheres as carriers |
| CN102807680A (en) * | 2012-07-16 | 2012-12-05 | 大连理工大学 | Preparation method and application of mono-(6-oxy-ethylenediamine tetraacetyl)-cyclodextrin cross-linked polymer |
| CN114674964A (en) * | 2022-05-26 | 2022-06-28 | 北京建筑大学 | Method for simultaneously measuring various thioether smelly substances in drinking water |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1128663C (en) * | 2002-07-18 | 2003-11-26 | 武汉大学 | Application of beta-cyclodextrin bonded silicone gel as solid phase extraction adsorption medium |
| CN1228121C (en) * | 2003-03-12 | 2005-11-23 | 武汉大学 | Extracting head for solid phase microextraction and its prepn and use |
-
2005
- 2005-11-14 CN CNB2005100197970A patent/CN100350995C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101992066A (en) * | 2010-09-02 | 2011-03-30 | 天津春发食品配料有限公司 | Beta-cyclodextrin substrate absorption material using glass microspheres as carriers |
| CN101992066B (en) * | 2010-09-02 | 2013-02-20 | 天津春发生物科技集团有限公司 | Beta-cyclodextrin substrate absorption material using glass microspheres as carriers |
| CN101972637A (en) * | 2010-09-29 | 2011-02-16 | 上海交通大学 | Triazines herbicide solid phase extraction tube and manufacturing method thereof |
| CN101972637B (en) * | 2010-09-29 | 2012-10-31 | 上海交通大学 | Triazines herbicide solid phase extraction tube and manufacturing method thereof |
| CN102807680A (en) * | 2012-07-16 | 2012-12-05 | 大连理工大学 | Preparation method and application of mono-(6-oxy-ethylenediamine tetraacetyl)-cyclodextrin cross-linked polymer |
| CN102807680B (en) * | 2012-07-16 | 2013-11-06 | 大连理工大学 | Preparation method and application of mono-(6-oxy-ethylenediamine tetraacetyl)-cyclodextrin cross-linked polymer |
| CN114674964A (en) * | 2022-05-26 | 2022-06-28 | 北京建筑大学 | Method for simultaneously measuring various thioether smelly substances in drinking water |
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| Publication number | Publication date |
|---|---|
| CN100350995C (en) | 2007-11-28 |
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