CN107126925A - A kind of novel magnetic nano material and its application in An Naigelieting drug tests - Google Patents
A kind of novel magnetic nano material and its application in An Naigelieting drug tests Download PDFInfo
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- CN107126925A CN107126925A CN201710440501.5A CN201710440501A CN107126925A CN 107126925 A CN107126925 A CN 107126925A CN 201710440501 A CN201710440501 A CN 201710440501A CN 107126925 A CN107126925 A CN 107126925A
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- Prior art keywords
- distilled water
- fullerene
- magnetic
- naigelieting
- ammoniacal liquor
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 30
- 238000003255 drug test Methods 0.000 title claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000012153 distilled water Substances 0.000 claims abstract description 51
- 229910003472 fullerene Inorganic materials 0.000 claims abstract description 38
- 238000001179 sorption measurement Methods 0.000 claims abstract description 33
- 239000007787 solid Substances 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 238000010992 reflux Methods 0.000 claims abstract description 22
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000004821 distillation Methods 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 9
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 9
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 claims abstract description 9
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 9
- 229910052786 argon Inorganic materials 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 36
- 239000000523 sample Substances 0.000 claims description 18
- 239000003814 drug Substances 0.000 claims description 17
- 238000002414 normal-phase solid-phase extraction Methods 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 14
- 239000006228 supernatant Substances 0.000 claims description 14
- 238000000926 separation method Methods 0.000 claims description 13
- 238000012360 testing method Methods 0.000 claims description 13
- 238000002604 ultrasonography Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000001514 detection method Methods 0.000 claims description 9
- 229940079593 drug Drugs 0.000 claims description 9
- 238000007865 diluting Methods 0.000 claims description 8
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical class [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 claims description 8
- 150000001805 chlorine compounds Chemical class 0.000 claims description 5
- 238000004062 sedimentation Methods 0.000 claims description 5
- 230000003139 buffering effect Effects 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000012488 sample solution Substances 0.000 claims description 3
- 241000872198 Serjania polyphylla Species 0.000 claims 2
- 150000001336 alkenes Chemical class 0.000 claims 2
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 claims 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 1
- 239000005864 Sulphur Substances 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 235000003891 ferrous sulphate Nutrition 0.000 claims 1
- 239000011790 ferrous sulphate Substances 0.000 claims 1
- 230000036571 hydration Effects 0.000 claims 1
- 238000006703 hydration reaction Methods 0.000 claims 1
- 239000000243 solution Substances 0.000 description 25
- 239000000047 product Substances 0.000 description 18
- 238000000034 method Methods 0.000 description 16
- 239000003463 adsorbent Substances 0.000 description 14
- 238000000605 extraction Methods 0.000 description 12
- 230000000694 effects Effects 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- 238000011084 recovery Methods 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 230000001934 delay Effects 0.000 description 5
- 239000007790 solid phase Substances 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 229910001873 dinitrogen Inorganic materials 0.000 description 4
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 4
- 238000005220 pharmaceutical analysis Methods 0.000 description 4
- 210000002966 serum Anatomy 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000002203 pretreatment Methods 0.000 description 3
- 238000000638 solvent extraction Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 229960000583 acetic acid Drugs 0.000 description 2
- 239000013060 biological fluid Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 239000012362 glacial acetic acid Substances 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 238000000622 liquid--liquid extraction Methods 0.000 description 2
- 238000001334 liquid-phase micro-extraction Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 235000017281 sodium acetate Nutrition 0.000 description 2
- 238000002470 solid-phase micro-extraction Methods 0.000 description 2
- BDKLKNJTMLIAFE-UHFFFAOYSA-N 2-(3-fluorophenyl)-1,3-oxazole-4-carbaldehyde Chemical compound FC1=CC=CC(C=2OC=C(C=O)N=2)=C1 BDKLKNJTMLIAFE-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 229940126678 chinese medicines Drugs 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000004255 ion exchange chromatography Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000002122 magnetic nanoparticle Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 238000004853 microextraction Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 230000004043 responsiveness Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- AYRVGWHSXIMRAB-UHFFFAOYSA-M sodium acetate trihydrate Chemical class O.O.O.[Na+].CC([O-])=O AYRVGWHSXIMRAB-UHFFFAOYSA-M 0.000 description 1
- 229940087562 sodium acetate trihydrate Drugs 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/405—Concentrating samples by adsorption or absorption
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Organic Chemistry (AREA)
- Biochemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Health & Medical Sciences (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Inorganic Chemistry (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The present invention relates to a kind of novel magnetic nano material and its application in An Naigelieting drug tests.The preparation method of novel magnetic nano material of the present invention comprises the following steps：(1) appropriate distilled water is taken, C is added70Fullerene, green vitriol, anhydrous ferric chloride, it is passed through nitrogen or argon gas was stirred after 15 20 minutes, is heated to reflux temperature, maintains the reflux for after 20 30 minutes, it is cooled to 85 90 DEG C, (85 90 DEG C) dropwise addition ammoniacal liquor of the temperature are maintained, continue the 1.5h of stirring reaction 1, reaction solution is in black cloudy state, naturally it is down to room temperature, stand after 0.5h, separated with magnet adsorption, obtain black solid；(2) black solid for obtaining step (1) is dried in vacuo 12 24h in 60 DEG C and is obtained black solid powder, as magnetic C with after distillation washing 35 times70Fullerene nanomaterial.
Description
Technical field
The invention belongs to material and Pharmaceutical Analysis field, and in particular to a kind of novel magnetic nano material and its in An Naige
Arrange the application in the drug test of spit of fland.
Background technology
Because the drug concentration in the drug concentration in organism, especially serum is directly related to drug effect.Therefore, from facing
For in terms of bed application and Drug safety assessment, it is necessary to set up a kind of simple, sensitive, accurate detection biological fluid and medicine
The analysis method of An Naigelieting contents in thing.There are high performance liquid chromatography, thin layer with extensive Pharmaceutical Analysis method at present
Chromatography, ion-exchange chromatography etc..Current few document reports on An Naigelieting content assaying methods, and use purple
The report that outside-visible spectrophotometry determines An Naigelieting contents there is no.
In Pharmaceutical Analysis, the separation and concentration for sample is that the pre-treatment of sample plays critical effect.Separation is rich
Collection is so that analysans is separated from its matrix, extracted, while reaching the purpose of concentration medicine, is carried so as to realize
High accuracy, the effect of sensitivity.With the development and progress in epoch, current separation and concentration technology has obtained very big development.
Conventional method for separating and concentrating has extraction, including liquid-liquid extraction (LLE), SPE (SPE), solid phase micro-extraction technique
(SPME), liquid-phase micro extraction technique (LPME), dispersive liquid-liquid microextraction technology (DLLME) etc..Surveyed to biological fluid
Regularly, because complicated component in body fluid, it is not readily separated to form interference, and medicament contg to be determined is general all very low, so sample
The separation and concentration of product seems increasingly important.Take reasonable efficient separation and concentration technology by the medicine to be measured of low content from complicated
Separation and Extraction comes out in biological substrate, for fast and accurately carrying out quantitative analysis, is the important content of internal Pharmaceutical Analysis.
In view of the advantage and disadvantage of various isolation technics, have very big improvement, such as Magnetic solid phases extraction skill for solid phase extraction techniques at present
Art.The solid phase extraction (SPE) grown up earliest is called Solid extraction column method, be from early 1970s grow up one
Plant sample separation and concentration technology.And Magnetic solid phases extraction be based on SPE and grow up it is a kind of new, environment-friendly
Sample pre-treatments analytical technology, utilizes the suction-operated more efficiently extractive analysis thing of magnetic Nano material.Magnetic Nano material
Because combining the dual characteristicses of magnetic responsiveness and nano-particle, so the adsorbent that can be extracted as Magnetic solid phases.With it is traditional
Sample Pretreatment Technique Used such as solid phase extraction, solvent extraction, ultrasonic extraction etc. compared, and Magnetic solid phases extraction is used in
The process of sample pre-treatments is largely simplified, and easily realizes the separation of phase.
Magnetic carrier technology (MCT) is reported by Robinson et al. first.In 1973, micro- (or nanometer) magnetic carrier
Synthesis has caused extensive interest.MCT unique and noticeable characteristic is that magnetic nanoparticle can be by applying
Easily separated from sample solution external magnetic field.These particles are superparamagnetism, it means that they can be easy
Ground is attracted to a magnet, but it is on the scene be removed after can not keep magnetic.The characteristic causes them to be particularly suitable for use in sample preparation, because
For that compared with non magnetic adsorbent, need not centrifuge after the extraction or filtered sample.
The content of the invention
The present invention provides a kind of magnetic C70Fullerene nanomaterial (is abbreviated as C70-Fe3O4), it is characterised in that its preparation side
Method comprises the following steps：
(1) appropriate distilled water is taken, C is added70Fullerene, green vitriol, anhydrous ferric chloride, are passed through nitrogen or argon
After gas agitating 15-20 minutes, reflux temperature is heated to, maintains the reflux for after 20-30 minutes, is cooled to 85-90 DEG C, the temperature is maintained
(85-90 DEG C) dropwise addition ammoniacal liquor, continues stirring reaction 1-1.5h, and reaction solution is in black cloudy state, and room temperature is down to naturally, is stood
After 0.5h, separated with magnet adsorption, obtain black solid；
(2) black solid for obtaining step (1) is dried in vacuo 12-24h in 60 DEG C and obtained with after distillation washing 3-5 times
Black solid powder, as magnetic C70Fullerene nanomaterial (is abbreviated as C70-Fe3O4)。
Distilled water, C in step (1)70Fullerene, green vitriol, anhydrous ferric chloride, the consumption of ammoniacal liquor are every
0.1mmol C are added in 100mL distilled water70Fullerene, 0.2mmol green vitriols, 0.4mmol anhydrous ferric chlorides, 3-
5mL ammoniacal liquor；The distilled water is preferably through the distilled water after ultrasound.
The present invention provides above-mentioned magnetic C70Fullerene nanomaterial (is abbreviated as C70-Fe3O4) preparation method, its feature exists
In comprising the following steps：
(1) appropriate distilled water is taken, C is added70Fullerene, green vitriol, anhydrous ferric chloride, are passed through nitrogen or argon
After gas agitating 15-20 minutes, reflux temperature is heated to, maintains the reflux for after 20-30 minutes, is cooled to 85-90 DEG C, the temperature is maintained
(85-90 DEG C) dropwise addition ammoniacal liquor, continues stirring reaction 1-1.5h, and reaction solution is in black cloudy state, and room temperature is down to naturally, is stood
After 0.5h, separated with magnet adsorption, obtain black solid；
(2) black solid for obtaining step (1) is dried in vacuo 12-24h in 60 DEG C and obtained with after distillation washing 3-5 times
Black solid powder, as magnetic C70Fullerene nanomaterial.
Distilled water, C in step (1)70Fullerene, green vitriol, anhydrous ferric chloride, the consumption of ammoniacal liquor are every
0.1mmol C are added in 100mL distilled water70Fullerene, 0.2mmol green vitriols, 0.4mmol anhydrous ferric chlorides, 3-
5mL ammoniacal liquor；The distilled water is preferably through the distilled water after ultrasound.
Above-mentioned magnetic C in another embodiment of the present invention70Fullerene nanomaterial (is abbreviated as C70-Fe3O4) peace how
Application in Ge Lieting drug tests.C70-Fe3O4Played a role as solid phase extraction adsorbentses.
Magnetic C70Fullerene nanomaterial C70-Fe3O4The purposes in An Naigelieting drug concentrations in detection sample, it is special
Levy and be to comprise the following steps：
(1) extract：In 10.0mL centrifuge tubes, it is separately added into the Acetic acid-sodium acetates of 1.0mL pH 3.0 (HAc-NaAc) and delays
Rush solution, appropriate testing sample solution, 10-20mg C70-Fe3O4, with distilled water diluting to 10mL, shake up, shake at room temperature
Swing after 10-15min, standing, C is separated with magnet adsorption70-Fe3O4, after after upper solution clear, taking supernatant with ultraviolet
Visible spectrophotometer is detected；
(2) elute：By step (1) the isolated C of magnet adsorption70-Fe3O4It is placed in centrifuge tube, adds anhydrous second
Alcohol, constant volume shakes up, at room temperature, vibrates after 20-30min, standing, makes C with magnet adsorption separation70-Fe3O4Sedimentation, treats upper strata
After solution clear, supernatant is taken to be detected with ultraviolet-uisible spectrophotometer.
Another embodiment of the present invention provides above-mentioned magnetic C70Fullerene nanomaterial C70-Fe3O4Preparing solid phase extraction
The application in adsorbent is taken, especially the application in being used to detect the solid phase extraction adsorbentses of An Naigelieting medicines is being prepared.
Constant volume of the present invention refers to solubilizer (absolute ethyl alcohol) to scale (centrifuge tube).
The advantage of the invention is that：1. magnetic C is prepared first70Fullerene nanomaterial C70-Fe3O4Inhaled as SPE
Attached dose is used for the detection of An Naigelieting medicines, C70-Fe3O4More general Magnetic solid phases extract adsorbent, with to An Naigelie
Spit of fland adsorptivity is strong, and the characteristics of easily elute；2. the C that the present invention is prepared70-Fe3O4Particle diameter utilizes C in 5-8nm70Caged
Structure can fully be contacted with An Naigelieting medicines, form π-pi-conjugated system, hydrogen bond etc..
Brief description of the drawings
Magnetic C prepared by Fig. 1 embodiments 170Fullerene nanomaterial (is abbreviated as C70-Fe3O4) TEM figure
The standard working curve of Fig. 2 An Naigelieting concentration and absorbance
Embodiment
For the ease of a further understanding of the present invention, examples provided below has done more detailed description to it.But
It is that these embodiments only are not used for limiting the scope of the present invention or implementation principle, reality of the invention for being better understood from invention
The mode of applying is not limited to herein below.
Embodiment 1
200mL distilled water is taken, 0.2mmol C are added70Fullerene, 0.4mmol green vitriols, 0.8mmol is anhydrous
Iron chloride, after being passed through nitrogen gas stirring 15 minutes, is heated to reflux temperature, maintains the reflux for after 20-30 minutes, is cooled to 85-90 DEG C,
Maintain (85-90 DEG C) of the temperature that ammoniacal liquor (6mL) is added dropwise, continue stirring reaction 1-1.5h, reaction solution is in black cloudy state, natural
Room temperature is down to, is stood after 0.5h, is separated with magnet adsorption, obtain black solid；After distillation washing 3-5 times, in 60 DEG C of vacuum
Dry 12h and obtain black solid powder, as magnetic C70Fullerene nanomaterial (is abbreviated as C70-Fe3O4, Fig. 1, hereinafter referred to as
Product A)；The distilled water used in the present embodiment is the distilled water after ultrasound.
Embodiment 2
100mL distilled water is taken, 0.1mmol C are added70Fullerene, 0.2mmol green vitriols, 0.4mmol is anhydrous
Iron chloride, after being passed through argon gas stirring 20 minutes, is heated to reflux temperature, maintains the reflux for after 20-30 minutes, be cooled to 85-90 DEG C,
Maintain (85-90 DEG C) of the temperature that ammoniacal liquor (5mL) is added dropwise, continue stirring reaction 1-1.5h, reaction solution is in black cloudy state, natural
Room temperature is down to, is stood after 0.5h, is separated with magnet adsorption, obtain black solid；After distillation washing 3-5 times, in 60 DEG C of vacuum
Dry 24h and obtain black solid powder, as magnetic C70Fullerene nanomaterial (is abbreviated as C70-Fe3O4, SEM figure with Fig. 1 mono-
Cause, hereinafter referred to as product B)；The distilled water used in the present embodiment is the distilled water after ultrasound.
Embodiment 3
200mL distilled water is taken, 0.2mmol graphenes, 0.4mmol green vitriols, the anhydrous chlorinations of 0.8mmol is added
Iron, after being passed through nitrogen gas stirring 15 minutes, is heated to reflux temperature, maintains the reflux for after 20-30 minutes, is cooled to 85-90 DEG C, maintenance
Ammoniacal liquor (6mL) is added dropwise in (85-90 DEG C) of the temperature, continues stirring reaction 1-1.5h, and reaction solution is in black cloudy state, is down to naturally
Room temperature, stands after 0.5h, is separated with magnet adsorption, obtain black solid；After distillation washing 3-5 times, in 60 DEG C of vacuum drying
12h obtains black solid powder, as magnetic graphene material (hereinafter referred to as products C)；The distilled water used in the present embodiment
For the distilled water after ultrasound.
Embodiment 4
200mL distilled water is taken, 0.4mmol green vitriols are added, 0.8mmol anhydrous ferric chlorides are passed through nitrogen and stirred
Mix after 15 minutes, be heated to reflux temperature, maintain the reflux for after 20-30 minutes, be cooled to 85-90 DEG C, maintain the temperature (85-90
DEG C) ammoniacal liquor (6mL) is added dropwise, continue stirring reaction 1-1.5h, reaction solution is in black cloudy state, and room temperature is down to naturally, is stood
After 0.5h, separated with magnet adsorption, obtain black solid；After distillation washing 3-5 times, it is dried in vacuo 12h in 60 DEG C and obtains black
Color solid powder, as magnetic Fe3O4Material (hereinafter referred to as product D)；The distilled water used in the present embodiment is after ultrasound
Distilled water.
Embodiment 5
200mL distilled water is taken, 0.4mmol C are added70Fullerene, 0.4mmol green vitriols, 0.8mmol is anhydrous
Iron chloride, after being passed through nitrogen gas stirring 15 minutes, is heated to reflux temperature, maintains the reflux for after 20-30 minutes, is cooled to 85-90 DEG C,
Maintain (85-90 DEG C) of the temperature that ammoniacal liquor (6mL) is added dropwise, continue stirring reaction 1-1.5h, reaction solution is in black cloudy state, natural
Room temperature is down to, is stood after 0.5h, is separated with magnet adsorption, obtain black solid；After distillation washing 3-5 times, in 60 DEG C of vacuum
Dry 12h and obtain black solid powder, as magnetic C70Fullerene nanomaterial (hereinafter referred to as product E)；Make in the present embodiment
Distilled water is the distilled water after ultrasound.
Embodiment 6
200mL distilled water is taken, 0.1mmol C are added70Fullerene, 0.4mmol green vitriols, 0.8mmol is anhydrous
Iron chloride, after being passed through nitrogen gas stirring 15 minutes, is heated to reflux temperature, maintains the reflux for after 20-30 minutes, is cooled to 85-90 DEG C,
Maintain (85-90 DEG C) of the temperature that ammoniacal liquor (6mL) is added dropwise, continue stirring reaction 1-1.5h, reaction solution is in black cloudy state, natural
Room temperature is down to, is stood after 0.5h, is separated with magnet adsorption, obtain black solid；After distillation washing 3-5 times, in 60 DEG C of vacuum
Dry 12h and obtain black solid powder, as magnetic C70Fullerene nanomaterial (hereinafter referred to as product F)；Make in the present embodiment
Distilled water is the distilled water after ultrasound.
The drafting of the standard working curve of embodiment 7
Reagent
An Naigelieting standard items (content ＞ 99.7%) and tablet (specification：100mg/ pieces) ring medicine company share is joined by Jiangsu
Co., Ltd provides；Methanol, ethanol, ammoniacal liquor, sodium acetate trihydrate, glacial acetic acid are bought in Chinese medicines group.All water are in experiment
High purity water, reagent is that analysis is pure.
An Naigelieting standard liquids (0.10mg/mL)：0.010g An Naigelieting standards are accurately weighed with assay balance
Product, 100mL is settled to distilled water dissolving, is placed in cool dark place and is preserved.
The cushioning liquid of pH 3.0：0.80g sodium acetate trihydrates are weighed, are dissolved with water, 5.4mL glacial acetic acid is added, it is dilute with water
500mL is released, is 3.0 in adjusting pH on acidometer.
Instrument
(Shimadzu instrument Suzhou is limited for SHIMADZU UV-1780 spectrophotometers (UV-VIS spectrophotometer)
Company), centrifuge TDL80-2B (Anting Scientific Instrument Factory, Shanghai)；Digital display thermostat water bath (Guo Hua Electrical Appliances Co., Ltd)；Very
Empty drying box (Shanghai Yiheng Scientific Instruments Co., Ltd)；(Shanghai is gloomy reliable to be tested DGG-9030B types electric heating constant-temperature blowing drying box
Instrument Ltd.)；PH S-25 types pH meter (upper Nereid section thunder magnetic)；Five side's KQ-50E ultrasonic cleaners.
Sample preparation
The preparation of An Naigelieting tablet samples：Take An Naigelieting tablet grind into powders, equivalent to 1 tablet medicine of correct amount
The powder of thing, is added in 100mL volumetric flasks, adds 50mL distilled water ultrasonic dissolutions so that tablet uniformly divides after all dissolving
Turbid solution is dissipated into, then 100mL is settled to distilled water, with 0.45 μm of membrane filtration, filtrate is taken in a dried and clean beaker,
5mL filtrates are measured with pipette in another 50mL volumetric flasks, are shaken up with being vibrated after distilled water constant volume.
The preparation of human blood final proof：The serum of healthy premenopausal volunteers is taken, is added after appropriate An Naigelieting standard liquids, by 1:4
Ratio add methanol remove serum in albumen, 4000r/min centrifuge 15min, take supernatant to analyze.
The drafting of standard working curve
Curve (Fig. 2), the analytical performance parameter determined are drawn to corresponding An Naigelieting concentration with absorption values
It the results are shown in Table 1.As shown in Table 1, the range of linearity is 0.10-2.5 μ g/mL, and detection is limited to 0.0926 μ g/mL.
The linear dimensions and test limit of the analysis method of table 1
Embodiment 8
Example 1
(1) extract：In 10.0mL centrifuge tubes, it is separately added into the Acetic acid-sodium acetates of 1.0mL pH 3.0 (HAc-NaAc) and delays
Product A prepared by solution, 20 μ L An Naigelieting standard liquids (0.10mg/mL), 10mg embodiments 1 is rushed, distilled water diluting is used
To 10mL, shake up, vibrate at room temperature after 10-15min, standing, with magnet adsorption separating and extracting adsorbent C70-Fe3O4, treat
After layer solution clear, supernatant is taken to be detected with ultraviolet-uisible spectrophotometer, testing result is less than the detection of working curve
Lower limit, i.e. An Naigelieting are almost entirely by C70-Fe3O4Absorption.
(2) elute：By step (1) the isolated extraction adsorbent C of magnet adsorption70-Fe3O4It is placed in 5mL centrifuge tubes
In, absolute ethyl alcohol is added, constant volume shakes up, at room temperature, vibrated after 20-30min, standing, make C with magnet adsorption separation70-
Fe3O4Sedimentation, after after upper solution clear, takes supernatant to be detected with ultraviolet-uisible spectrophotometer, testing result is scaled
0.3931 μ g/mL (the μ g/mL of theoretical value 0.40).
Example 2
(1) extract：In 10.0mL centrifuge tubes, it is separately added into the Acetic acid-sodium acetates of 1.0mL pH 3.0 (HAc-NaAc) and delays
Product B prepared by solution, 20 μ L An Naigelieting standard liquids (0.10mg/mL), 20mg embodiments 2 is rushed, distilled water diluting is used
To 10mL, shake up, vibrate at room temperature after 10-15min, standing, with magnet adsorption separating and extracting adsorbent C70-Fe3O4, treat
After layer solution clear, supernatant is taken to be detected with ultraviolet-uisible spectrophotometer, testing result is less than the detection of working curve
Lower limit, i.e. An Naigelieting are almost entirely by C70-Fe3O4Absorption.
(2) elute：By step (1) the isolated extraction adsorbent C of magnet adsorption70-Fe3O4It is placed in 5mL centrifuge tubes
In, absolute ethyl alcohol is added, constant volume shakes up, at room temperature, vibrated after 20-30min, standing, make C with magnet adsorption separation70-
Fe3O4Sedimentation, after after upper solution clear, takes supernatant to be detected with ultraviolet-uisible spectrophotometer, testing result is scaled
0.3929 μ g/mL (the μ g/mL of theoretical value 0.40).
Example 3
Extraction：In 10.0mL centrifuge tubes, the Acetic acid-sodium acetates of 1.0mL pH 3.0 (HAc-NaAc) buffering is separately added into molten
Products C prepared by liquid, 20 μ L An Naigelieting standard liquids (0.10mg/mL), 10mg embodiments 3, with distilled water diluting extremely
10mL, shakes up, and vibrates at room temperature after 10-15min, standing, with magnet adsorption separating and extracting adsorbent, treats that upper solution is clarified
After transparent, supernatant is taken to be detected with ultraviolet-uisible spectrophotometer, testing result is scaled 0.1654 μ g/mL, illustrates products C pair
An Naigelieting adsorption effect is general, is not suitable for the solid phase extraction adsorbentses in An Naigelieting drug tests.
Example 4
Extraction：In 10.0mL centrifuge tubes, the Acetic acid-sodium acetates of 1.0mL pH 3.0 (HAc-NaAc) buffering is separately added into molten
Product D prepared by liquid, 20 μ L An Naigelieting standard liquids (0.10mg/mL), 10mg embodiments 4, with distilled water diluting extremely
10mL, shakes up, and vibrates at room temperature after 10-15min, standing, with magnet adsorption separating and extracting adsorbent, treats that upper solution is clarified
After transparent, supernatant is taken to be detected with ultraviolet-uisible spectrophotometer, testing result is scaled 0.2218 μ g/mL, illustrates D pairs of product
An Naigelieting adsorption effect is general, is not suitable for the solid phase extraction adsorbentses in An Naigelieting drug tests.
Example 5
(1) extract：In 10.0mL centrifuge tubes, it is separately added into the Acetic acid-sodium acetates of 1.0mL pH 3.0 (HAc-NaAc) and delays
Product E prepared by solution, 20 μ L An Naigelieting standard liquids (0.10mg/mL), 10mg embodiments 5 is rushed, distilled water diluting is used
To 10mL, shake up, vibrate at room temperature after 10-15min, standing, with magnet adsorption separating and extracting adsorbent C70-Fe3O4, treat
After layer solution clear, supernatant is taken to be detected with ultraviolet-uisible spectrophotometer, testing result is less than the detection of working curve
Lower limit, i.e. An Naigelieting are almost entirely by C70-Fe3O4Absorption.
(2) elute：By step (1) the isolated extraction adsorbent C of magnet adsorption70-Fe3O4It is placed in 5mL volumetric flasks
In, absolute ethyl alcohol is added, constant volume shakes up, at room temperature, vibrated after 20-30min, standing, make C with magnet adsorption separation70-
Fe3O4Sedimentation, after after upper solution clear, takes supernatant to be detected with ultraviolet-uisible spectrophotometer, testing result is scaled
0.3288 μ g/mL (the μ g/mL of theoretical value 0.40).Illustrate product E adsorption effect preferably, but it elutes desorption effect and paid no attention to
Think, be not suitable for the solid phase extraction adsorbentses in An Naigelieting drug tests.
Example 6
(1) extract：In 10.0mL centrifuge tubes, it is separately added into the Acetic acid-sodium acetates of 1.0mL pH 3.0 (HAc-NaAc) and delays
Product F prepared by solution, 20 μ L An Naigelieting standard liquids (0.10mg/mL), 10mg embodiments 6 is rushed, distilled water diluting is used
To 10mL, shake up, vibrate at room temperature after 10-15min, standing, with magnet adsorption separating and extracting adsorbent C70-Fe3O4, treat
After layer solution clear, supernatant is taken to be detected with ultraviolet-uisible spectrophotometer, testing result is scaled 0.1258 μ g/mL,
Illustrate that product F is undesirable to An Naigelieting adsorption effect, be not suitable for the solid phase extraction in An Naigelieting drug tests
Take adsorbent.
Embodiment 9
An Naigelieting concentration and the standard working curve of absorbance that the present invention is made using embodiment 7, using ultraviolet
The precision of An Naigelieting concentration and reappearance, the degree of accuracy and the investigation of the rate of recovery in visible spectrophotometer detection sample.
Precision and reappearance
Compound concentration is the An Naigelieting standard liquids of 0.40,0.80 μ g/mL, two kinds of concentration respectively, and withinday precision is
The sample of same concentration is continuously analyzed 5 times on the same day, precision is calculated, it is 0.07%~0.21% as a result to show RSD, is represented
Preferably, this method can be used for routine analysis to the reappearance of method.
In this experiment, An Naigelieting tablets are determined with working curve method, are as a result 101.5mg/ pieces, with
There was no significant difference for labelled amount 100mg/ pieces.
The degree of accuracy and the rate of recovery
The method tested in this experiment using mark-on determines the rate of recovery, and have rated the degree of accuracy of method.Relative recovery
It is calculated as follows：
C in formulareal、Cadded、CfoundIt is the An Naigelieting concentration determined in actual sample respectively, is added in sample
An Naigelieting concentration of standard solution, An Naigelieting concentration in the sample determined after standard items is added.Measuring result
As shown in table 2.The rate of recovery is 96.8%~102.3% in medicine, and the rate of recovery is 96.8%~100.9%, explanation in human serum
The accuracy of method is preferable, the measure available for An Naigelieting contents in medicine.
The rate of recovery of table 2 is tested
It can be seen that, the method that the present invention detects An Naigelieting concentration in sample using ultraviolet-uisible spectrophotometer is accurate
Degree is high, favorable reproducibility, and testing result is credible in embodiment 8.
Claims (8)
1. a kind of magnetic C70Fullerene nanomaterial, it is characterised in that its preparation method comprises the following steps：
(1) appropriate distilled water is taken, C is added70Fullerene, green vitriol, anhydrous ferric chloride, are passed through nitrogen or argon gas is stirred
Mix after 15-20 minutes, be heated to reflux temperature, maintain the reflux for after 20-30 minutes, be cooled to 85-90 DEG C, maintain the temperature (85-
90 DEG C) ammoniacal liquor is added dropwise, continue stirring reaction 1-1.5h, reaction solution is in black cloudy state, and room temperature is down to naturally, stands 0.5h
Afterwards, separated with magnet adsorption, obtain black solid；
(2) black solid for obtaining step (1) is dried in vacuo 12-24h in 60 DEG C and is obtained black with after distillation washing 3-5 times
Solid powder, as magnetic C70Fullerene nanomaterial (is abbreviated as C70-Fe3O4)。
2. the magnetic C described in claim 170Fullerene nanomaterial, it is characterised in that distilled water, C in the step (1)70It is rich
It is per addition 0.1mmol C in 100mL distilled water to strangle alkene, green vitriol, anhydrous ferric chloride, the consumption of ammoniacal liquor70Fowler
Alkene, 0.2mmol green vitriols, 0.4mmol anhydrous ferric chlorides, 3-5mL ammoniacal liquor；After the distilled water is preferably through ultrasound
Distilled water.
3. the magnetic C described in claim any one of 1-270The preparation method of fullerene nanomaterial, it is characterised in that including such as
Lower step：
(1) appropriate distilled water is taken, C is added70Fullerene, green vitriol, anhydrous ferric chloride, are passed through nitrogen or argon gas is stirred
Mix after 15-20 minutes, be heated to reflux temperature, maintain the reflux for after 20-30 minutes, be cooled to 85-90 DEG C, maintain the temperature (85-
90 DEG C) ammoniacal liquor is added dropwise, continue stirring reaction 1-1.5h, reaction solution is in black cloudy state, and room temperature is down to naturally, stands 0.5h
Afterwards, separated with magnet adsorption, obtain black solid；
(2) black solid for obtaining step (1) is dried in vacuo 12-24h in 60 DEG C and is obtained black with after distillation washing 3-5 times
Solid powder, as magnetic C70Fullerene nanomaterial.
4. the preparation method described in claim 3, it is characterised in that distilled water, C in the step (1)70Fullerene, seven hydration sulphur
Sour ferrous iron, anhydrous ferric chloride, the consumption of ammoniacal liquor are per addition 0.1mmol C in 100mL distilled water70Fullerene, the water of 0.2mmol seven
Close ferrous sulfate, 0.4mmol anhydrous ferric chlorides, 3-5mL ammoniacal liquor；The distilled water is preferably through the distilled water after ultrasound.
5. the magnetic C described in claim any one of 1-270Fullerene nanomaterial answering in An Naigelieting drug tests
With.
6. the application described in claim 5, it is characterised in that the magnetic C70Fullerene nanomaterial is adsorbed as SPE
Agent plays a role.
7. the magnetic C described in claim any one of 1-270Fullerene nanomaterial An Naigelieting medicines in detection sample are dense
Purposes in degree, it is characterised in that comprise the following steps：
(1) extract：In 10.0mL centrifuge tubes, the Acetic acid-sodium acetates of 1.0mL pH 3.0 (HAc-NaAc) buffering is separately added into molten
Liquid, appropriate testing sample solution, 10-20mg C70-Fe3O4, with distilled water diluting to 10mL, shake up, vibrate at room temperature
After 10-15min, standing, C is separated with magnet adsorption70-Fe3O4, after after upper solution clear, take supernatant with it is ultraviolet can
See that spectrophotometer is detected；
(2) elute：By step (1) the isolated C of magnet adsorption70-Fe3O4It is placed in centrifuge tube, adds absolute ethyl alcohol, it is fixed
Hold, shake up, at room temperature, vibrate after 20-30min, standing, make C with magnet adsorption separation70-Fe3O4Sedimentation, treats upper solution
After clear, supernatant is taken to be detected with ultraviolet-uisible spectrophotometer.
8. the magnetic C described in claim any one of 1-270Fullerene nanomaterial answering in solid phase extraction adsorbentses are prepared
With the especially application in preparing for detecting the solid phase extraction adsorbentses of An Naigelieting medicines.
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| CN104258807A (en) * | 2014-10-13 | 2015-01-07 | 中国环境科学研究院 | Magnetic nano material solid phase extracting agent as well as preparation method and application thereof |
| CN104785197A (en) * | 2014-01-16 | 2015-07-22 | 中国药科大学 | Preparation method of mixed hemi-micelle solid phase extractant based on Fe3O4 magnetic nanoparticles |
| CN105854796A (en) * | 2016-04-08 | 2016-08-17 | 济南大学 | Preparation method and application of magnetic bimetallic oxide/carbon composite material |
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| CN104785197A (en) * | 2014-01-16 | 2015-07-22 | 中国药科大学 | Preparation method of mixed hemi-micelle solid phase extractant based on Fe3O4 magnetic nanoparticles |
| CN104258807A (en) * | 2014-10-13 | 2015-01-07 | 中国环境科学研究院 | Magnetic nano material solid phase extracting agent as well as preparation method and application thereof |
| CN105854796A (en) * | 2016-04-08 | 2016-08-17 | 济南大学 | Preparation method and application of magnetic bimetallic oxide/carbon composite material |
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| JOSE A. RODRIGUEZ 等: "Magnetic solid phase extraction based on fullerene and activated carbon adsorbents for determination of azo dyes in water samples by capillary electrophoresis", 《ANALYTICAL METHODS》 * |
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