CN108889284A - A kind of shell-core structure magnetic microsphere and its extracting process to clenbuterol hydrochloride in mutton - Google Patents

A kind of shell-core structure magnetic microsphere and its extracting process to clenbuterol hydrochloride in mutton Download PDF

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CN108889284A
CN108889284A CN201810766552.1A CN201810766552A CN108889284A CN 108889284 A CN108889284 A CN 108889284A CN 201810766552 A CN201810766552 A CN 201810766552A CN 108889284 A CN108889284 A CN 108889284A
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extraction
clenbuterol hydrochloride
shell
mutton
clenbuterol
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CN108889284B (en
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连丽丽
张鑫洋
娄大伟
王希越
李玉莹
吕进义
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Jilin Institute of Chemical Technology
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Abstract

The invention discloses a kind of shell-core structure magnetic Nano microsphere and its to the extracting process of clenbuterol hydrochloride in mutton, wherein the magnetic Nano microsphere is Fe3O4@C@Co3O4, the present invention is based on Magnetic solid phases abstraction technique, using the magnetic Nano microsphere as adsorbent, extracts to the clenbuterol hydrochloride in mutton, realizes the selective enrichment to clenbuterol hydrochloride in meat samples to be measured, be remarkably improved high performance liquid chromatography（Equipped with UV detector）The sensitivity that clenbuterol hydrochloride in mutton is detected.

Description

A kind of shell-core structure magnetic microsphere and its extracting process to clenbuterol hydrochloride in mutton
Technical field
The invention belongs to technical field of food detection, in particular to a kind of shell-core structure magnetic microsphere and its in mutton The extracting process of clenbuterol hydrochloride.
Background technique
Check that the report of clenbuterol hydrochloride occurs often in the meats such as some pigs, sheep, ox recent years, the rank and file gets over More to pay close attention to the hygienic manufacturing conditions of some meats and its meat products.It is serious bad anti-that clenbuterol hydrochloride is that one kind can cause human body The feed addictive answered, if poisoning or even the phenomena of mortality can be generated after the exceeded meat products of people's large amounts of food.How quickly, The content of clenbuterol hydrochloride becomes people's question of common concern in effective detection meat.
Due to meat matrix complexity, and the content of clenbuterol hydrochloride is usually trace level, it is therefore desirable to carry out pre-treatment to sample. That there are organic solvent consumptions is big, specificity is not strong due to traditional solid phase extraction column, price and is used only once Problem needs to develop, preparation method simple, cheap, selective novel extraction material strong to clenbuterol hydrochloride accumulation ability Material.So a kind of efficient, quick, convenient and fast novel sample pretreatment-magnetic solid phase extraction technology, increasingly causes people Concern.
Summary of the invention
Extraction the object of the present invention is to provide a kind of magnetic Nano microsphere of shell-core structure and its to clenbuterol hydrochloride in mutton Method.It can realize that the extraction of clenbuterol hydrochloride in meat samples, cooperation chromatography are real using the shell-core structure magnetic Nano microsphere Quick, the Sensitive Detection of trace clenbuterol hydrochloride in existing mutton.
The purpose of the present invention is what is be achieved through the following technical solutions：
Weigh the magnetic Nano microsphere of modified carbon shell（Fe3O4@C）, ultrapure water, dehydrated alcohol, butanol, cobalt nitrate, lemon is added Mixture is transferred in the hydrothermal synthesis kettle of 50mL to after mixing, is placed in baking oven and is heated to by sour sodium and urea, ultrasound 120℃.To after reaction, Magnetic Isolation black solid, as magnetic Fe3O4@C@Co3O4。
Further, the preparation method is further comprising the steps of：The Fe that will be prepared3O4@C@Co3O4, successively use After water, dehydrated alcohol sufficiently wash, then carry out vacuum drying treatment.
It is another object of the present invention to what is be achieved through the following technical solutions：
A method of using clenbuterol hydrochloride in above-mentioned magnetic Nano microsphere extraction mutton, include the following steps：
Using the clenbuterol hydrochloride in dehydrated alcohol ultrasonic extraction mutton, the sample solution containing clenbuterol hydrochloride is obtained, is dried with nitrogen, it is ultrapure Water constant volume, then with hydrochloric acid or sodium hydroxide solution tune pH to 9, obtain extracting solution；
Said extracted liquid 10mL is taken, shell-core structure magnetic adsorbent Fe described in claim 1 is added3O4@C@Co3O4, whirlpool Rotation extraction, Magnetic Isolation have loaded the adsorbent of clenbuterol hydrochloride, discard supernatant liquid；Eluent is added and is vortexed again for elution, magnetic point From, pipette supernatant and be dried with nitrogen under water-bath, that is, complete clenbuterol hydrochloride extraction, carried out after being settled to certain volume with ultrapure water Chromatography.
Further, the magnetic microsphere Fe3O4@C@Co3O4Additive amount be 0.5-3mg//mL.Preferably, additive amount For 1.5mg/mL.
Further, with hydrochloric acid or sodium hydroxide solution tune pH to 9.
Further, the time of vortex extraction is 5-30min every time.Preferably, be vortexed extraction 20min every time.
Further, the eluent is acetic acid：Methanol=15%：85%, vortex elution time is 5-20min, preferred whirlpool Rotation elution 10min.
The present invention having the beneficial effect that compared with prior art：
1, magnetic Nano microsphere Fe of the present invention3O4@C@Co3O4In shell-core structure, partial size 100-150nm, C@Co3O4 Fe has been arrived by successfully package3O4Surface is uniformly distributed the mesoporous of about 5nm, and center is wrapped in Fe3O4；
2, by Fe3O4@C@Co3O4With do not modify Co3O4Magnetic microsphere Fe3O4@C compares the rate of recovery of clenbuterol hydrochloride, Shell-core structure magnetic Nano microsphere Fe of the present invention3O4@C@Co3O4It is best to the extraction ability of clenbuterol hydrochloride in extracting solution；
3, by shell-core structure magnetic Nano microsphere Fe of the present invention3O4@C@Co3O4As adsorbent, the Optimized Extraction time, The conditions such as system pH, effluent volume, elution time extract the clenbuterol hydrochloride in mutton, realize to clenbuterol hydrochloride in mutton Selective extraction, to improve the sensitivity that liquid chromatogram detects clenbuterol hydrochloride；
Although 4, carbon material also has certain extracting power to clenbuterol hydrochloride, it, which is extracted, does not have selectivity, and modifies Co3O4The magnetic Nano microsphere of shell makes its extraction have certain choosing by metal and the intermolecular coordination of clenbuterol hydrochloride Selecting property reduces the interference of background, and chromatographic peak is apparent, interference is few, utilizes Fe3O4@C@Co3O4Magnetic dispersion extraction sample is molten Clenbuterol hydrochloride in liquid is conducive to the abundant effect of adsorbent and target molecule, and Solid Phase Extraction is also not present（SPE）Pillar is easy hair The problem of raw column blocking, there is apparent advantage.
Detailed description of the invention
Fig. 1 is the results of FT-IR schematic diagram of the magnetic microsphere；
Wherein, a-Fe3O4, b-Fe3O4@C, c-Fe3O4@C@Co3O4；
Fig. 2 is the XRD result schematic diagram of the magnetic microsphere；
Fig. 3 is the TEM result schematic diagram under the different amplification of the magnetic microsphere；
Wherein, A-0.2 μm, B-20nm；
Fig. 4 is influence schematic diagram of the adsorbent mass to extraction efficiency；
Fig. 5 is influence schematic diagram of the adsorption time to extraction efficiency；
Fig. 6 is influence schematic diagram of the different pH to extraction efficiency；
Fig. 7 is influence schematic diagram of the different elution times to extraction efficiency；
Fig. 8 is influence schematic diagram of the different effluent volumes to extraction efficiency；
Fig. 9 is schematic diagram of the different magnetic microspheres to clenbuterol hydrochloride extraction efficiency；
Wherein, 1- Fe3O4@C, 2-Fe3O4@C@Co3O4。
Specific embodiment
The main agents and instrument used：
Ultra Performance Liquid Chromatography instrument UPLC (H-Class, Waters instrument company of the U.S.)；Micro-whirlpool mixed instrument（Shanghai Hu Xi Analysis instrument Co., Ltd., Factory）；Clenobuterol hydrochloride analytical standard product（German DR）；Ractopamine, husky butanol amine analysis mark Quasi- product（Sigma Aldrich）.
Embodiment 1
A kind of shell-core structure magnetic Nano microsphere and preparation method thereof is present embodiments provided, the magnetic Fe of 0.2g is weighed3O4@ The cobalt nitrate of 11.6mL ultrapure water, 8.3mL dehydrated alcohol, 0.1mL butanol, 0.291g is added in C（1mmoL）, 0.1g citric acid Sodium（Na3Cit）With the urea of 0.16g, mixture is transferred in the hydrothermal synthesis kettle of 50mL, is placed in after mixing by ultrasound 120 DEG C are heated in baking oven.After reacting 8h, by magnetic Fe3O4@C@Co3O4It is separated by magnet, through ultrapure water and anhydrous second After alcohol sufficiently washs, it is dry to be placed in 60 DEG C of vacuum oven.
Hereinafter, passing through infrared spectroscopy, X-ray diffraction（XRD）, transmission electron microscope（TEM）The methods of characterization magnetic Fe3O4@C@ Co3O4Physical and chemical performance.
As shown in Figure 1, as shown in a, it can be observed that Fe3O4Fe-O key in crystal is in 591cm-1There are stronger spies at place Levy absorption peak；B is Fe3O4@C infrared spectrogram, it can be observed that in 3450cm-1There is a strong absorption peak at place, is attributed to hydroxyl Characteristic absorption, in 1600cm-1The strong absworption peak that place occurs belongs to the stretching vibration of carboxyl, this illustrates that carbon shell is successfully repaired It adorns in Fe3O4The surface of magnetic microsphere, c Fe3O4@C@Co3O4Infrared spectrogram, in 665cm-1There is an absorption peak at place, ownership In the absorption peak of Co-O key.
By in Fig. 2 it is found that XRD is the result shows that product has a Fe simultaneously3O4And Co3O4Characteristic diffraction peak.
By A in Fig. 3 it is found that Fe3O4@C@Co3O4It is dispersed preferable, spherical in shape, shell-core structure, diameter 100-150nm. By B in Fig. 2 it is found that Fe3O4@C@Co3O4There are uniform nano pores on surface.
Embodiment 2
The shell-core structure magnetic Nano microsphere Fe that the present embodiment is prepared using embodiment 13O4@C@Co3O4It extracts in mutton The method of clenbuterol hydrochloride, includes the following steps：
Using the clenbuterol hydrochloride in 30mL dehydrated alcohol ultrasonic extraction 10g mutton, the sample solution containing clenbuterol hydrochloride is obtained, nitrogen is blown Dry, ultrapure water is settled to 50mL, then with hydrochloric acid or sodium hydroxide solution tune pH to 9, obtains extracting solution；
Said extracted liquid 10mL is taken, magnetic adsorbent Fe described in claim 1 is added3O4@C@Co3O4 20mg, be vortexed extraction It takes 20min, Magnetic Isolation to load the adsorbent of clenbuterol hydrochloride, discards supernatant liquid；Eluent acetic acid is added：Methanol=15%：85% washes De- liquid 3mL is vortexed again for elution 10min, Magnetic Isolation, pipettes supernatant and be dried with nitrogen under water-bath, be settled to ultrapure water Chromatography is carried out after 1mL.
Embodiment 3
Investigate magnetic microsphere Fe3O4@C@Co3O4Influence of the dosage to clenbuterol hydrochloride extraction efficiency in mutton.
According to the clenbuterol hydrochloride in 2 the method for embodiment extraction mutton, difference is, magnetic microsphere Fe3O4@C@Co3O4's Additive amount is respectively 5,10,15,20,30mg.As shown in figure 4, in magnetic microsphere Fe3O4@C@Co3O4When quality is 20mg, to three Person has preferable extraction efficiency, and therefore, the optimum absorbent quality that the present invention selects is 20mg.
Embodiment 4
Investigate influence of the different adsorption times to clenbuterol hydrochloride extraction efficiency in extraction mutton.
According to the clenbuterol hydrochloride in 2 the method for embodiment extraction mutton, difference is, adsorption time is respectively 5,10,15, 20,25,30 min.As shown in Figure 5, when adsorption time reaches 20min, the extraction efficiency of three reaches maximum, therefore this The adsorption time that invention selects is 20min.
Embodiment 5
Different system pH are investigated to magnetic microsphere Fe3O4@C@Co3O4Extract the influence of clenbuterol hydrochloride extraction efficiency in mutton.
According to the clenbuterol hydrochloride in 2 the method for embodiment extraction mutton, difference is that sample solution pH value is adjusted to respectively 3,5,7,9,11.As shown in fig. 6, magnetic microsphere is maximum to the extraction efficiency of three kinds of clenbuterol hydrochlorides when pH is 9, present invention selection System pH=9.
Embodiment 6
Investigate influence of the different elution times to clenbuterol hydrochloride extraction efficiency in extraction mutton.
According to the clenbuterol hydrochloride in 2 the method for embodiment extraction mutton, difference is, elution time is respectively 2,5,10, 20 min.As shown in Figure 7, the elution time of three kinds of target analytes extraction efficiency in 10min has had reached maximum value, this Invention selection elution 10min.
Embodiment 7
Investigate influence of the different effluent volumes to clenbuterol hydrochloride extraction efficiency in extraction mutton.
According to the clenbuterol hydrochloride in 2 the method for embodiment extraction mutton, difference is, the volume of eluent is respectively 1,2, 3,4 mL.As shown in Figure 8, when effluent volume is 3mL, extraction efficiency reaches maximum.Therefore, elution process of the present invention is added Effluent volume be 3mL.
Comparative example
In order to prove, Co3O4Effect in adsorbent preparation, is prepared for Fe3O4@C magnetic microsphere, weighs the magnetism of 0.23g Fe3O4, the glucose of 1.8g and the ultrapure water of 40mL is added, ultrasound closes the hydro-thermal that mixture is transferred to 50mL to after mixing 180 DEG C are heated in kettle, being placed in baking oven.After reacting 8h, magnetic Fe can be obtained3O4@C, by magnetic Fe3O4@C passes through After sufficiently being washed with ultrapure water and dehydrated alcohol, it is dry to get the magnetism for arriving black to be placed in 60 DEG C of vacuum oven for Magneto separate Fe3O4@C。
In order to ensure prepared Fe3O4@C@Co3O4Really effective to the enrichment of clenbuterol hydrochloride and extraction and and intermediate product Compared to best, use Fe3O4@C and magnetic Nano microsphere Fe described in embodiment 13O4@C@Co3O4Extraction efficiency into Comparison is gone.In the identical situation of the experiment condition of two kinds of magnetic Nano materials, data cases are as shown in figure 9, Fe3O4@C@ Co3O4Show stronger extracting power.
Confirm the Fe by shell-core structure of the present invention3O4@C@Co3O4Can have to the clenbuterol hydrochloride in mutton Effect, selective enrichment, and clenbuterol hydrochloride is adsorbed on magnetic material, has been transferred to lesser solution environmental later In the middle, it was demonstrated that the present invention is in selective enrichment and detects and obtains ideal effect in mutton in terms of clenbuterol content.

Claims (7)

1. weighing magnetic Fe3O4Ultrapure water, dehydrated alcohol, butanol, cobalt nitrate, sodium citrate and urea is added in@C, ultrasonic to mixed After closing uniformly, mixture is transferred in the hydrothermal synthesis kettle of 50mL, is placed in baking oven and is heated to 120 DEG C, certain time to be reacted Afterwards, product is separated by magnet after cooling, after ultrapure water and dehydrated alcohol sufficiently wash, 60 DEG C of vacuum drying obtain shell- Core-shell structure magnetic adsorbent Fe3O4@C@Co3O4。
2. a kind of shell-core structure magnetic Nano microsphere, which is characterized in that the shell-core structure magnetic Nano microsphere is wanted by right Preparation method described in asking 1 is made.
3. a kind of utilize three kinds of trace clenbuterol hydrochlorides in shell-core structure magnetic Nano microsphere extraction mutton as claimed in claim 2 Method, three kinds of trace clenbuterol hydrochlorides are clenobuterol hydrochloride（Clenbuterol）, Ractopamine（Ractopamine）, it is husky Butanolamine（Salbutamol）, the described method comprises the following steps：
Using the clenbuterol hydrochloride in dehydrated alcohol ultrasonic extraction mutton, the sample solution containing clenbuterol hydrochloride is obtained, is dried with nitrogen, it is ultrapure Water constant volume, then with hydrochloric acid or sodium hydroxide solution tune pH to 9, obtain extracting solution；
Said extracted liquid 10mL is taken, shell-core structure magnetic adsorbent Fe described in claim 1 is added3O4@C@Co3O4, it is vortexed Extraction, Magnetic Isolation have loaded the adsorbent of clenbuterol hydrochloride, discard supernatant liquid；Eluent is added and is vortexed again for elution, Magnetic Isolation, Supernatant is pipetted to be dried with nitrogen under water-bath, that is, complete clenbuterol hydrochloride extraction, prepare after being settled to certain volume with ultrapure water into Row chromatography.
4. the method for clenbuterol hydrochloride in extraction mutton according to claim 3, which is characterized in that the shell-core structure is magnetic Microballoon Fe3O4@C@Co3O4Additive amount be 0.5-3mg/mL.
5. the method for clenbuterol hydrochloride in extraction mutton according to claim 3, which is characterized in that use hydrochloric acid or sodium hydroxide Solution tune pH to 9.
6. the method for clenbuterol hydrochloride in extraction mutton according to claim 6, which is characterized in that the time for the extraction that is vortexed every time For 5-30min.
7. the method for clenbuterol hydrochloride in extraction mutton according to claim 6, which is characterized in that elution time 5-20min.
CN201810766552.1A 2018-07-13 2018-07-13 Shell-core structure magnetic microsphere and extraction method of clenbuterol from mutton by using same Active CN108889284B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105301152A (en) * 2015-11-02 2016-02-03 重庆医科大学 Biocompatible solid-phase extraction method suitable for clebuterol
CN106345477A (en) * 2016-08-23 2017-01-25 江苏大学 Preparation method and application of magnetic Fe3O4@C/Co3O4 composite light catalyst
CN106526166A (en) * 2015-09-15 2017-03-22 陈军 Rapid detection of lean meat powder in pork

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106526166A (en) * 2015-09-15 2017-03-22 陈军 Rapid detection of lean meat powder in pork
CN105301152A (en) * 2015-11-02 2016-02-03 重庆医科大学 Biocompatible solid-phase extraction method suitable for clebuterol
CN106345477A (en) * 2016-08-23 2017-01-25 江苏大学 Preparation method and application of magnetic Fe3O4@C/Co3O4 composite light catalyst

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