CN101239254B - Mycotoxin purification column and mycotoxin purification method - Google Patents
Mycotoxin purification column and mycotoxin purification method Download PDFInfo
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- CN101239254B CN101239254B CN2008100611194A CN200810061119A CN101239254B CN 101239254 B CN101239254 B CN 101239254B CN 2008100611194 A CN2008100611194 A CN 2008100611194A CN 200810061119 A CN200810061119 A CN 200810061119A CN 101239254 B CN101239254 B CN 101239254B
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Abstract
The present invention provides a mycotoxin purifying column filled with composite fillings and its purifying method. The purifying column mainly includes a column, a filling material filled in the column and the a sieve plate set on the two ends of the filling material, the filling material is layered, being a super cell, a neutral alumina and a silica gel in turns up and down, the filling grain diameter is 5-100 mu m. The purifying method of the invention uses adsorption theory of the sorbent filling material, selectively absorbs impurity in flowing extracting solution by utilizing filling material, flushes purifying column by eluent, collects sample effluent liquid and eluent. Impurity absorbs on the column, achiving the effect of removing impurity. The advantages of the mycotoxin purifying column are the lower cost, convenient producing, and changable filling ratio if needed; the purifying method has a quick speed, wide application, convenient operation, better purifying effect.
Description
(1) technical field
The present invention relates to a kind of mycotoxin decontaminating column, and the method for utilizing this mycotoxin decontaminating column that mycotoxin in the sample is purified.
(2) background technology
It is to pollute and residual mycotoxin in order accurately to detect in food, the feed in the down-stream that mycotoxin in food and the feed extract is purified, carrying out various decontaminating columns and purification method that this purification adopts at present exists the processing time long, be of limited application, shortcomings such as cost is higher, and clean-up effect is unsatisfactory.
(3) summary of the invention
The object of the invention provides a kind of cheap, mycotoxin that can purify multiple class simultaneously, and the decontaminating column of ideal purification effect, and the method for utilizing this mycotoxin decontaminating column that mycotoxin in the sample is purified.
The technical solution used in the present invention is:
A kind of mycotoxin decontaminating column, mainly comprise cylinder, be seated in the filler in the cylinder and be arranged on the filler sieve plate at two ends up and down, it is characterized in that: described filler layering filling, be followed successively by from top to bottom: filter aid, neutral alumina, silica gel, filler granularity are 5～100 μ m.
Concrete, described packing quality consists of: filter aid 5～50%, neutral alumina 5～90%, silica gel 5～90%.
Described filter aid is this area filter aid commonly used, and as super-cell or pearlite filtering aid etc., the present invention is preferably super-cell, and described super-cell is preferably: Celite545, Celite-hyflosuper-cell or ZX-616 etc.
Preferably, described cylinder volume is 0.1～1000mL, and internal diameter is 1～50mm.
Preferred described plate thickness is 0.5～5mm, diameter and cylinder internal diameter coupling, and the aperture in described sieve plate hole, the particularly aperture in lower end sieve plate hole are less than packing material size, and the aperture in sieve plate hole is 1～100 μ m usually.
The preferred described packing quality of the present invention consists of: super-cell 10%, neutral alumina 20～60%, silica gel 30～70%.
The invention still further relates to a kind of mycotoxin purification method of mycotoxin decontaminating column, described method is as follows: be that eluent carries out wash-out to the extract that contains mycotoxin with the polar organic solvent, isolate mycotoxin, described polar organic solvent is methyl alcohol, acetonitrile or ethyl acetate.Described polar organic solvent is preferably acetonitrile.
The described acquisition that contains the extract of mycotoxin: with the aqueous solution of acetonitrile volumetric concentration 10～20%, extract mycotoxin in the sample, obtain containing the extract of mycotoxin.
In the whole process, flow rate of liquid preferably is controlled at and is no more than 4ml/min.
Beneficial effect of the present invention is mainly reflected in:
1. adopt mycotoxin decontaminating column of the present invention, wash-out separates, and can be apace the extract of food and feed be carried out purification separation, and the whole operation process is no more than 20 minutes;
2. the present invention adopts different filler configurations to be applicable to that (when sample was corn flour, peanut butter, paddy: silica gel reduced for the sample of different substrates, different types of mycotoxin, aluminium oxide increases), applied widely, good purification satisfies the analysis requirement to different types of sample, different types of mycotoxin;
3. the filler of the present invention's use is common chemical substance, and stable in properties is with low cost, is easy to make and preserve, and is convenient to use.
(4) description of drawings
The mycotoxin decontaminating column structure side view that Fig. 1 relates to for the embodiment of the invention 1.
The mycotoxin decontaminating column structure vertical view that Fig. 2 relates to for the embodiment of the invention 1.
Fig. 3 carries out the chromatogram of sample analysis after the purified treatment for embodiment 1.
Fig. 4 is embodiment 4 clean-up effects chromatograms relatively; A: handle B without decontaminating column: handle through decontaminating column.
(5) specific embodiment
The present invention is described further below in conjunction with specific embodiment, but protection scope of the present invention is not limited in this:
Mycotoxin decontaminating column structure of the present invention is referring to Fig. 1～2, decontaminating column monnolithic case syringe-like bucket, and it is by cylinder 1, upper sieve plate 2, sieve plate 3 and place up and down that the filler between the sieve plate 4,5,6 constitutes down.The cylinder volume is 6cc, filler 2.5g, and particle size range is at 5～100 microns.The thickness of upper sieve plate 1 and following sieve plate 2 is 2 millimeters, and the mesh-structured physicochemical properties on it are stable, can rise and filter and iris action, prevents that filler from coming out, and stops big particle diameter material to enter.The mechanism of action of mycotoxin decontaminating column of the present invention is to utilize the absorption of compounded mix, filtration (salification, hydrogen bond, coordination etc.), impurity is optionally adsorbed, keeps, in purification process, utilize suitable eluting solvent that small part is adsorbed target analytes and elute.
Embodiment 1:
Thing to be checked: peanut butter;
Mycotoxin type: aflatoxin;
Decontaminating column filler configuration: filler 2.5g, silica gel (Qingdao wave silica-gel desiccant factory) 1.35g wherein, neutral alumina (Zhengzhou English promise chromatography experiment technology Co., Ltd) 0.9g, filter aid (diatomite ZX-616, the bright clean Pu Dao in Beijing Filtertek Inc.) 0.25g;
Purification method comprises the following steps:
The first step, the preparation sample solution extracts target analytes in the peanut butter at twice with 20ml acetonitrile/water (v/v:10/90) mixed liquor, the merging extract;
In second step, last sample is got extract 2ml and is added in the decontaminating column, collects to flow out liquid;
The 3rd step was that eluent carries out wash-out with methyl alcohol, flow through decontaminating column with the 4ml acetonitrile, drained under the negative pressure, collected to flow out liquid;
The analyte rate of recovery: target analytes is 17 kinds of mycotoxins, adopts the LC-MS instrument to detect, and chromatogram is seen Fig. 3.85～101%, relative standard deviation: less than 5%.
Embodiment 2:
Thing to be checked: paddy;
Mycotoxin type: aflatoxin, the trichothecene same clan;
Decontaminating column filler configuration: filler 2.5g, silica gel 0.9g wherein, neutral alumina 1.35g, filter aid (diatomite Celite545, Merck chemical industry technology (Shanghai) company) 0.25g;
Purification method comprises the following steps:
The first step, the preparation sample solution extracts analyte in the paddy at twice with 20ml acetonitrile/water (v/v:16/84) mixed liquor, the merging extract;
In second step, last sample is got extract 2ml and is added in the decontaminating column, collects to flow out liquid;
The 3rd step was that eluent carries out wash-out with the acetonitrile, flow through decontaminating column with the 4ml acetonitrile, drained under the negative pressure, collected to flow out liquid;
The analyte rate of recovery: 90～105%, relative standard deviation: less than 5%.
Embodiment 3:
Thing to be checked: corn flour;
Mycotoxin contamination type: the trichothecene same clan;
Decontaminating column filler configuration: filler 2.5g, silica gel 1.8g wherein, neutral alumina 0.45g, filter aid (Celite-hyflosuper-cell, Merck chemical industry technology (Shanghai) company) 0.25g;
Purification method comprises the following steps:
The first step, the preparation sample solution extracts analyte in the corn at twice with 20ml acetonitrile/water (v/v:20/80) mixed liquor, the merging extract;
In second step, last sample is got extract 2ml and is added in the decontaminating column, collects to flow out liquid;
The 3rd step was that eluent carries out wash-out with ethyl acetate, flow through decontaminating column with the 4ml acetonitrile, blotted under the negative pressure, collected to flow out liquid;
The analyte rate of recovery: 82～98%, relative standard deviation: less than 5%.
Embodiment 4: compliance test result
Thing to be checked: paddy;
Mycotoxin type: aflatoxin, the trichothecene same clan;
Get same sample, A handles the direct injected chromatographic isolation without this patent decontaminating column; B is a sample introduction chromatographic isolation again after this patent decontaminating column is handled, and the configuration of decontaminating column filler is implemented according to embodiment 2 with purification method.
In this embodiment, handle through decontaminating column, impurity absorption is on decontaminating column, and analyte flows out along with flowing out liquid.The decontaminating column treatment effect is can't see tangible chromatographic peak without the sample that decontaminating column is handled because of impurity disturbs referring to Fig. 4.
Claims (8)
1. mycotoxin decontaminating column, mainly comprise cylinder, be seated in the filler in the cylinder and be arranged on the filler sieve plate at two ends up and down, it is characterized in that: described filler layering filling, be followed successively by from top to bottom: filter aid, neutral alumina and silica gel, packing material size are 5～100 μ m; Described packing quality consists of: filter aid 5～50%, neutral alumina 5～90%, silica gel 5～90%.
2. mycotoxin decontaminating column as claimed in claim 1 is characterized in that described filter aid is a super-cell.
3. mycotoxin decontaminating column as claimed in claim 2 is characterized in that described super-cell is Celite545, Celite-hyflosuper-cell or ZX-616.
4. as the described mycotoxin decontaminating column of one of claim 1～3, it is characterized in that described plate thickness is 0.5～5mm, the aperture in sieve plate hole is less than packing material size.
5. mycotoxin decontaminating column as claimed in claim 1 is characterized in that described packing quality consists of: super-cell 10%, neutral alumina 20～60%, silica gel 30～70%.
6. mycotoxin purification method of utilizing the described mycotoxin decontaminating column of claim 1, described method is to be that eluent carries out wash-out to the extract that contains mycotoxin with the polar organic solvent, isolate mycotoxin, described polar organic solvent is methyl alcohol, acetonitrile or ethyl acetate.
7. method as claimed in claim 6 is characterized in that described polar organic solvent is an acetonitrile.
8. method as claimed in claim 6 is characterized in that the described extract that contains mycotoxin is the aqueous solution with acetonitrile volumetric concentration 10～20%, extracts mycotoxin in the sample, obtains containing the extract of mycotoxin.
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| CN2008100611194A CN101239254B (en) | 2008-03-12 | 2008-03-12 | Mycotoxin purification column and mycotoxin purification method |
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| CN2008100611194A CN101239254B (en) | 2008-03-12 | 2008-03-12 | Mycotoxin purification column and mycotoxin purification method |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2012007503A1 (en) * | 2010-07-14 | 2012-01-19 | Qiagen Gmbh | New storage, collection or isolation device |
| JP6161205B2 (en) * | 2010-07-14 | 2017-07-12 | キアゲン ゲーエムベーハー | Device for the isolation and / or purification of biomolecules |
| CN102401820A (en) * | 2011-11-21 | 2012-04-04 | 江苏省农业科学院 | Method for detecting content of mycotoxins in wheat |
| CN103263888B (en) * | 2013-05-31 | 2015-04-22 | 浙江省疾病预防控制中心 | Column for separating and purifying micromolecular pollutant in food and application method thereof |
| CN104258596A (en) * | 2014-09-25 | 2015-01-07 | 上海市农业科学院 | Solid-phase extraction column for enriching and purifying deoxidized nivalenol |
| CN106267891B (en) * | 2015-06-03 | 2023-06-06 | 中美华世通生物医药科技(武汉)股份有限公司 | Method for rapid separation and purification of compound |
| CN105092353B (en) * | 2015-07-17 | 2017-10-03 | 丁葵英 | A kind of recoverying and utilizing method of residues of pesticides QuEChERS purified powders |
| CN105092352B (en) * | 2015-07-17 | 2017-09-26 | 郭礼强 | A kind of recoverying and utilizing method of mycotoxin QuEChERS purified powders |
| CN113413638A (en) * | 2021-05-31 | 2021-09-21 | 青岛科技大学 | A chromatography purification column for azithromycin production is with methyl alcohol purification |
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