CN109557223A - QuEChERs pillar and its application - Google Patents
QuEChERs pillar and its application Download PDFInfo
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- CN109557223A CN109557223A CN201811535178.0A CN201811535178A CN109557223A CN 109557223 A CN109557223 A CN 109557223A CN 201811535178 A CN201811535178 A CN 201811535178A CN 109557223 A CN109557223 A CN 109557223A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention provides a kind of QuEChERs pillars, use anhydrous magnesium sulfate and amino multi-wall carbon nanotube for filler.Purposes in terms of interfering matrix in removal meat sample the present invention also provides QuEChERs pillar.The present invention also provides the minimizing technologies that matrix is interfered in a kind of meat sample, using QuEChERs pillar above-mentioned.QuEChERs pillar of the invention can effectively remove the interference matrix such as moisture, fat, polypeptide in meat sample, to realize the enrichment of other trace materials in meat.
Description
Technical field
The present invention relates to agricultural product security detection technique field, in particular it relates to a kind of QuEChERs pillar and
It is applied.
Background technique
Meat products will usually carry out the detection of trace materials such as residue of veterinary drug before entering market sale.But meat
Class product, such as beef, wherein there is very strong matrix effect, seriously affect containing interfering substances such as a large amount of fat, albumen
The detection of trace materials in meat products.Currently, mainly there is admittedly the minimizing technology of the interfering substances such as fat, albumen in beef sample
The several methods such as phase extraction, Solid-phase Microextraction, liquid-liquid extraction method, accelerated solvent extraction follow the example of, matrix solid phase dispersion method, these
Traditional sample preparation methods can be competent at basic beef sample pre-treatment demand to a certain extent.But for sensitive
Degree and the high detection of precise requirements, these conventional methods tend not to meet the requirements.
QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) is newest hair in the world in recent years
A kind of quick sample pretreatment technology for detection of agricultural products that exhibition is got up, is taught by United States Department of Agriculture Anastassiades
Equal to exploitation in 2003.Principle is similar to high performance liquid chromatography (HPLC) and Solid Phase Extraction (SPE), is filled out using adsorbent
Material and the interaction and impurities in matrix, adsorbing contaminant is to achieve the purpose that impurity and purification.QuEChERS method has following excellent
Gesture: (1) rate of recovery is high, is greater than 85% to the rate of recovery of a large amount of polarity and volatile pesticide species；(2) accuracy and accuracy
Height can be corrected with internal standard method；(3) analyzable pesticide range is wide, including polarity, nonpolar pesticide variety can utilize
This technology obtains the preferable rate of recovery；(4) analysis speed is fast, and the processing of 6 samples can be completed in 30min；(5) solvent uses
Amount is few, pollute it is small, it is cheap and do not use chloride solvent；(6) easy to operate, without well trained and just compared with high professional qualification
It can complete well；(7) acetonitrile seals immediately after being added to container, reduces the touch opportunity of itself and staff；(8) sample system
Seldom glassware is used during standby, device is simple.
Currently, the QuEChERS pillar that QuEChERS method uses is usually using carbon nanotube as filler.Multi-walled carbon nanotube
Have many advantages, such as that surface has hydrophobicity, large specific surface area.It can be to meat sample by the extraction column of filler of multi-walled carbon nanotube
Fat and the impurity such as albumen in product carry out good absorption, simultaneously for other trace materials such as residue of veterinary drug etc. absorption compared with
It is small, it is suitable for the enrichment analysis of other trace materials.But in high-precision detection, individually using carbon nanotube as the small of filler
Column is unable to satisfy high-precision requirement.
Summary of the invention
Goal of the invention of the invention is provided a kind of for meat matrix purification for the deficiencies in the prior art
QuEChERs pillar and its application.
On the one hand, the present invention provides a kind of QuEChERs pillars, using anhydrous magnesium sulfate and amination multi-wall carbon nano-tube
Pipe is filler.
Further, the weight ratio of anhydrous magnesium sulfate and amino multi-wall carbon nanotube is 3-5:4-6.
Further, the weight ratio of anhydrous magnesium sulfate and amino multi-wall carbon nanotube is 4:5.
On the other hand, in terms of interfering matrix in removal meat sample the present invention provides above-mentioned QuEChERs pillar
Purposes.
Further, the meat sample is selected from beef, mutton, pork, chicken and duck.
Further, the interference matrix includes moisture, fatty acid and polypeptide.
On the other hand, the present invention provides the minimizing technologies that matrix is interfered in a kind of meat sample, using above-mentioned
QuEChERs pillar.
Further, which includes:
N-hexane is added into the meat sample blended and shakes homogeneous, acetonitrile mixing is then added, is centrifugally separating to obtain and mentions
Take liquid；
Demulsifier, liquid separation after concussion mixing are added into extracting solution, obtained clear liquid is eluted by QuEChERs pillar, washed
It is stand-by after de- liquid filtering.
Compared with the prior art, technical solution of the present invention has the following beneficial effects:
It is good that QuEChERs pillar of the invention can interfere matrix to carry out moisture, fat, the polypeptide etc. in meat sample
Good absorption, the absorption simultaneously for other trace materials such as residue of veterinary drug etc. is smaller, is suitable for the enrichment of other trace materials
Analysis.The QuEChERs pillar can greatly improve the impurity purification efficiency of meat sample, reduce trace materials in meat sample
The time of pre-treatment operation and cost.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of QuEChERs pillar of the invention.
Specific embodiment
In order to fully understand the purpose of the present invention, feature and effect, by following specific embodiments, the present invention is made detailed
It describes in detail bright.For process of the invention in addition to following the description, remaining is all made of the conventional method or device of this field.Unless otherwise
Illustrate, otherwise the term involved in the present invention all has the normally understood meaning of those skilled in the art.
At present individually using multi-walled carbon nanotube as filler QuEChERs pillar there are aiming at the problem that, it is of the invention
Inventor improves filler, is provided a kind of QuEChERs pillar, use anhydrous magnesium sulfate and amination by research
Multi-walled carbon nanotube is filler.
In QuEChERs pillar of the invention, the weight ratio of anhydrous magnesium sulfate and amino multi-wall carbon nanotube is 3-5:
4-6.Preferably, the weight ratio of anhydrous magnesium sulfate and amino multi-wall carbon nanotube is 4:5.
QuEChERs pillar of the invention is using the combination of anhydrous magnesium sulfate and amino multi-wall carbon nanotube as filler.
The moisture in meat sample substrate can be removed using anhydrous magnesium sulfate.Since the fatty acid in meat sample substrate contains carboxylic
The amino of base, amino multi-wall carbon nanotube can be in conjunction with carboxyl, to remove the rouge in meat sample to the full extent
Fat acid.It, can be with protein in adsorbing base and more also, since amino multi-wall carbon nanotube has very big specific surface area
Peptide.
QuEChERs pillar of the invention can use conventional structure, be made of known materials.A kind of optional structure shape
Formula is as shown in Figure 1, include filling column tube 1, upper sieve plate 2, mixed filler layer 3, lower sieve plate 4.Wherein, mixed filler layer 3 is by nothing
Water magnesium sulfate and amino multi-wall carbon nanotube mix according to the above ratio；The volume for filling column tube 1 is 1 to 10mL；Filler
The sieve plate of upper and lower ends, i.e. upper sieve plate 2 and lower sieve plate 4, can be made, thickness can be 2 to 5mm, hole of conventional material
Diameter can be 0.45 μm.
QuEChERs pillar of the invention can be made of method commonly employed in the art.
On the other hand, the use in terms of interfering matrix in removal meat sample the present invention provides above-mentioned QuEChERs pillar
On the way.Wherein, meat sample can be beef, mutton, pork, chicken and duck；Interference matrix includes moisture, fatty acid (or rouge
Fat) and polypeptide (or protein) etc..
On the other hand, the present invention provides the minimizing technologies that matrix is interfered in a kind of meat sample, using this method by meat
After interfering matrix removal and purification in class sample, the trace materials such as veterinary drug in meat sample can be made with further detection.
Specifically, the minimizing technology of interference matrix includes: in meat sample of the invention
S1 is extracted: n-hexane being added into the meat sample blended and shakes homogeneous, acetonitrile mixing, centrifugation point is then added
From obtaining extracting solution；
Purification: S2 demulsifier is added into extracting solution, liquid separation after concussion mixing, it is small that obtained clear liquid passes through QuEChERs
Column elution, it is stand-by after eluent filtering.
In S1 extraction step, meat sample, n-hexane, the ratio between acetonitrile can be 5 grams of meat samples: 25~
30ml n-hexane: 25~30ml acetonitrile.
In S1 extraction step, n-hexane is added into the meat sample blended can shake 10~30 points of homogeneous later
Clock；Acetonitrile is added later can be 1~3 minute with vortex mixed.
In S2 purifying step, demulsifier can be lauryl alcohol polyoxyethylene phosphate.
The filtrate that S2 purifying step obtains is i.e. for the use of subsequent detection of veterinary drugs in food.
Interfere various reagents used by the minimizing technology of matrix that can pass through conventional city in meat sample of the invention
Purchase obtains.
Embodiment
The present invention is further illustrated below by the mode of embodiment, but does not therefore limit the present invention to the reality
It applies among a range.In the following examples, the experimental methods for specific conditions are not specified, according to conventional methods and conditions, or according to quotient
The selection of product specification.
Embodiment 1
QuEChERs pillar includes filling column tube 1, upper sieve plate 2, mixed filler layer 3, lower sieve plate 4 in embodiment 1.Packed column
1 volume of pipe is 3mL；Upper sieve plate 2 and lower sieve plate 4 are polyethylene sieve plates, and thickness is 2mm respectively, and aperture is 0.45 μm；Mixed fillers
Layer 3 is by 120mg anhydrous magnesium sulfate (Kai Lida Chemical Co., Ltd.) and (the Shanghai spectrum vibration life of 150mg amino multi-wall carbon nanotube
Object Science and Technology Ltd.) it mixes.
Purification is removed to the interference matrix in beef using the QuEChERs pillar of embodiment 1, is specifically included:
S1: carrying out cutting for beef sample and blend, and takes the hamburger sample of 5.00g to be placed in 100ml tool plug centrifuge tube and adds
25~30ml n-hexane shakes homogeneous 10~30 minutes, adds 25~30ml acetonitrile, vortex mixed 1~3 minute, centrifugation divided
From being concentrated and be settled to 50ml.
S2: taking the resulting extracting solution of 20mL S1 step, and the demulsification such as lauryl alcohol polyoxyethylene phosphate is added thereto
Agent, concussion mixing, liquid separation, resulting clear liquid are transferred on QuEChERs pillar, and eluent is collected after elution；In 50 DEG C of water-baths
It is blown to nitrogen and is closely done, 5mL acetonitrile is added, after mixing on turbine mixer, filtrate is obtained by miillpore filter.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any substitutions made without departing from the spirit and principles of the present invention, combination, change, are simplified modification
Deng should be equivalent substitute mode, be included within the scope of the present invention.
Claims (8)
1. a kind of QuEChERs pillar, which is characterized in that use anhydrous magnesium sulfate and amino multi-wall carbon nanotube for filler.
2. QuEChERs pillar according to claim 1, which is characterized in that anhydrous magnesium sulfate and amination multi-wall carbon nano-tube
The weight ratio of pipe is 3-5:4-6.
3. QuEChERs pillar according to claim 2, which is characterized in that anhydrous magnesium sulfate and amination multi-wall carbon nano-tube
The weight ratio of pipe is 4:5.
4. purposes of the described in any item QuEChERs pillars of claims 1 to 3 in removal meat sample in terms of interference matrix.
5. purposes according to claim 4, which is characterized in that the meat sample is selected from beef, mutton, pork, chicken
And duck.
6. purposes according to claim 4, which is characterized in that the interference matrix includes moisture, fatty acid and polypeptide.
7. interfering the minimizing technology of matrix in a kind of meat sample, which is characterized in that using described in any one of claims 1 to 3
QuEChERs pillar.
8. interfering the minimizing technology of matrix in meat sample according to claim 7 characterized by comprising
N-hexane is added into the meat sample blended and shakes homogeneous, acetonitrile mixing is then added, is centrifugally separating to obtain extracting solution；
Demulsifier, liquid separation after concussion mixing are added into extracting solution, obtained clear liquid is eluted by QuEChERs pillar, eluent
It is stand-by after filtering.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811535178.0A CN109557223A (en) | 2018-12-14 | 2018-12-14 | QuEChERs pillar and its application |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811535178.0A CN109557223A (en) | 2018-12-14 | 2018-12-14 | QuEChERs pillar and its application |
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| CN109557223A true CN109557223A (en) | 2019-04-02 |
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| CN201811535178.0A Pending CN109557223A (en) | 2018-12-14 | 2018-12-14 | QuEChERs pillar and its application |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110243955A (en) * | 2019-05-20 | 2019-09-17 | 兰韬 | It is exclusively used in the QuEChERS purification pipe and application method of interference component in removal tealeaves and tobacco leaf |
| CN111203186A (en) * | 2020-01-14 | 2020-05-29 | 中国计量科学研究院 | Efficient purifying agent with self-separation function and preparation method and application thereof |
Citations (2)
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| CN103055540A (en) * | 2012-12-28 | 2013-04-24 | 中国农业大学 | Method for purifying pesticide residues and special purifier thereof |
| CN105259277A (en) * | 2015-07-23 | 2016-01-20 | 中国科学院西北高原生物研究所 | Method for detecting residual quantity of 18 sulfanilamide drugs in beef and mutton |
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2018
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103055540A (en) * | 2012-12-28 | 2013-04-24 | 中国农业大学 | Method for purifying pesticide residues and special purifier thereof |
| CN105259277A (en) * | 2015-07-23 | 2016-01-20 | 中国科学院西北高原生物研究所 | Method for detecting residual quantity of 18 sulfanilamide drugs in beef and mutton |
Non-Patent Citations (5)
| Title |
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| BINGQI ZHU ET AL.: "Simultaneous determination of 131 pesticides in tea by on-line GPC-GC–MS/MS using graphitized multi-walled carbon nanotubes as dispersive solid phase extraction sorbent", 《FOOD CHEMISTRY》 * |
| PENGYUE ZHAO ET AL.: "Multi-walled carbon nanotubes as alternative reversed-dispersive solid phase extraction materials in pesticide multi-residue analysis with QuEChERS method", 《JOURNAL OF CHROMATOGRAPHY A》 * |
| 余斐: "多壁碳纳米管在烟草多农药残留分析中的应用研究", 《万方平台》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110243955A (en) * | 2019-05-20 | 2019-09-17 | 兰韬 | It is exclusively used in the QuEChERS purification pipe and application method of interference component in removal tealeaves and tobacco leaf |
| CN110243955B (en) * | 2019-05-20 | 2022-06-14 | 北京科德诺思技术有限公司 | QuEChERS (QuEChERS) purifying tube special for removing interference components in tea leaves and tobacco leaves and application method |
| CN111203186A (en) * | 2020-01-14 | 2020-05-29 | 中国计量科学研究院 | Efficient purifying agent with self-separation function and preparation method and application thereof |
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