CN104645666B - A kind of nitric acid oxidation processing method of nano-graphite carbon black - Google Patents
A kind of nitric acid oxidation processing method of nano-graphite carbon black Download PDFInfo
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- CN104645666B CN104645666B CN201410645941.0A CN201410645941A CN104645666B CN 104645666 B CN104645666 B CN 104645666B CN 201410645941 A CN201410645941 A CN 201410645941A CN 104645666 B CN104645666 B CN 104645666B
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Abstract
The invention discloses the nitric acid oxidation processing method of a kind of nano-graphite carbon black, the method comprises the steps: take nano-graphite carbon black and the mixed liquor of nitric acid and heat, obtain aaerosol solution and layering is precipitated layer, in the beds of precipitation add with water and heat and static placement until solution be layered, the beds of precipitation after repeatedly being washed and the layering solution of the supernatant also carry out washing and separate, layering solution is filtered, it is dried in an oven, obtains the nano-graphite carbon black after final nitric acid oxidation processes.Operating process of the present invention is simple, it is applied widely that filler configuration is applicable to the sample of different substrates, different types of mycotoxin, good purification, filler processes through special process, after structure of modification, the selective cleaning of contratoxin sample has well effect, and effect of compounded mix serves more optimal effect to the purification of object.
Description
Technical field
The present invention relates to the nitric acid oxidation processing method of a kind of nano-graphite carbon black.
Background technology
Mycotoxin has been a global hot issue to the pollution of grain, feedstuff.The mycotoxin being currently known is up to hundreds of kind, and food, feedstuff, beverage, medical material industry endangers bigger being mainly with aflatoxin (Aflatoxin), ochratoxin A (Ochratoxin A), trichothecene (Trichothecenes), 6-(10-hydroxy-6-oxo-trans-1-undecenyl)-.beta.-resorcylic acid lactone (Zearalenone), FT (Fumonisin) and moniliformin (Moniliformin) occur more, owing to mycotoxin is of a great variety, structure complexity is various, pollution to food and feed is more and more extensive, detection by quantitative to mycotoxin becomes one of our important problem of puzzlement for a long time, the most at present that purified treatment rapidly and efficiently is particularly important.
In order to ensure the mycotoxin polluting and remaining in follow-up accurate analysis food, feedstuff, it is necessary to extract is carried out purify concentrate, current various solid-phase extraction columns and immune affinity column carry out purified treatment exist complex operation, pollute greatly, the poorest, the longest；The especially the highest testing cost causing enterprise and country's quality inspection organization of immune affinity column purification cost remains high, and directly contributes these purification methods.Long in the time of process, it is of limited application, relatively costly, the shortcomings such as clean-up effect is unsatisfactory.
Summary of the invention
It is an object of the invention to provide the nitric acid oxidation processing method of a kind of nano-graphite carbon black, solve the shortcoming that prior art exists.
The present invention adopts the following technical scheme that realization:
The nitric acid oxidation processing method of a kind of nano-graphite carbon black, it is characterised in that the method comprises the steps:
(1) 100g nano-graphite carbon black and 500mL nitric acid are taken；
(2) mixed liquor is heated in reflux boiling lasting 8h, obtain aaerosol solution；
(3) by the most static for this suspension placement until solution layering, draw the supernatant and be precipitated layer；
(4) adding the water with supernatant equivalent, ebuillition of heated 1h in the beds of precipitation, obtain suspension, static placement is until solution is layered；
(5) step (3), (4) it are iteratively repeated, the beds of precipitation after repeatedly being washed and the layering solution of the supernatant；
(6) this layering solution carries out in centrifuge washing to separate, until the pH value of the supernatant keeps constant；
(7) being filtered by the layering solution obtained in step 6, the nano-graphite carbon black obtained after filtration is dried in an oven, obtains the nano-graphite carbon black after final nitric acid oxidation processes.
Further, in step (1), the mass fraction of nitric acid is 40%.
A kind of sample purification processing method of trichothecene, it is characterized in that, the step of the method is: carry out extraction process for extract to containing mycotoxin sample with a certain proportion of organic solution, filtrate is purified by trichothecene decontaminating column, isolate mycotoxin after filtration.
Further, described organic solution is methanol or acetonitrile.
Using the Multifunctional cleanup column of the present invention, eluting separates, it is possible to the extracting solution to food and feedstuff carries out purification separation rapidly, and whole operating process is less than 20 minutes；The present invention uses different filler configurations to be applicable to the sample of different substrates, different types of mycotoxin (when sample is Semen Maydis powder, peanut butter, Oryza glutinosa: silica gel is less, aluminium oxide increases), applied widely, good purification, meets different types of sample, the analysis requirement of different types of mycotoxin；The filler that the present invention uses is general chemical material, and stable in properties, it is easy to manufacture and preserve is convenient to use；The filler of the present invention processes through special process, and after structure of modification, the selective cleaning of contratoxin sample has well effect, and effect of compounded mix serves more optimal effect to the purification of object.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of decontaminating column chromatograph packing material hierarchy.
Fig. 2 is solution collection of illustrative plates before and after grain class sample purification.
Fig. 3 is sample solution collection of illustrative plates of sample introduction chromatography again after this patent decontaminating column processes.
Detailed description of the invention
By the following description to embodiment; to more contribute to the public understanding present invention; but the specific embodiment given by applicant can't be considered as the restriction to technical solution of the present invention, any definition to parts or technical characteristic be changed and/or overall structure is made form and immaterial conversion is regarded as the protection domain that technical scheme is limited.
As shown in Figure 1 to Figure 3, trichothecene decontaminating column, including a cylinder 1, the bottom of cylinder 1 is scavenging solution reservoir 2, the lower end of cylinder 1 is provided with composite interstitial substance filler 3, is provided with a check valve 5 below composite interstitial substance filler 3, is provided with a liquid storage pipe 6 in the lower section of check valve 5, liquid storage pipe 6 is unstressed configuration liquid storage pipe in the present embodiment, is provided with extract in this unstressed configuration liquid storage pipe.
A kind of trichothecene composite interstitial substance filler, composite interstitial substance filler includes: nano-graphite carbon black, aluminium oxide, Aluminosilicates adsorbent and silica gel, filler granularity is between 5～100 μm, and quality group is proportional is: nano-graphite carbon black 5～50%, aluminium oxide 5～90%, Aluminosilicates adsorbent 5～90%.Silica gel 5～90%.
The nitric acid oxidation processing method of a kind of nano-graphite carbon black, the method comprises the steps:
(1) 100g nano-graphite carbon black and 500mL nitric acid are taken
(2) mixed liquor is heated in reflux boiling lasting 8h, obtain aaerosol solution；
(3) by the most static for this suspension placement until solution layering, draw the supernatant and be precipitated layer；
(4) adding the water with supernatant equivalent, ebuillition of heated 1h, (the most violent) in the beds of precipitation, obtain suspension, static placement is until solution is layered；
(5) step (3), (4) it are iteratively repeated, the beds of precipitation after repeatedly being washed and the layering solution of the supernatant；
(6) this layering solution carries out in centrifuge washing to separate, until the pH value of the supernatant keeps constant；
(7) being filtered by the layering solution obtained in step 6, the nano-graphite carbon black obtained after filtration is dried in an oven, obtains the nano-graphite carbon black after final nitric acid oxidation processes.
In another embodiment, in step (1), the mass fraction of nitric acid is 40%.
Silica gel treatment method in another embodiment: obtain the golden nanometer particle of 10-15nm diameter by reduction of sodium citrate gold chloride method, separately take 50um full multi-hole blangel and join in reactor, sequentially add dimethylbenzene 30ml, hydrosulphonyl silane reagent 20ml, pyridine 15ml heating reflux reaction was lowered the temperature after 24 hours, with toluene, dichloromethane, methanol, washing with acetone product post-drying, add in another reactor, add the golden nanometer particle originally prepared, add the positive stearylmercaptan of excess, heating reflux reaction 48 hours, product filters and with methanol, acetone washes post-drying, obtain.
A kind of sample purification processing method of trichothecene, the step of the method is: carry out extraction process for extract to containing mycotoxin sample with a certain proportion of organic solution, after filtration, filtrate is purified by trichothecene decontaminating column, isolate mycotoxin.
In another embodiment, organic solution is methanol or acetonitrile.
Application Example 1:
In Semen Maydis, DON NIV detects (200 column purification)
Filler configuring condition: the layering filling of described filler includes nano-graphite carbon black, superfine aluminium oxide, Aluminosilicates adsorbent, silica gel, and filler granularity is between 5～500 μm.
The detection of vomitoxin etc. in grain Semen Maydis:
Thing grain class such as Semen Maydis to be checked
Mycotoxin type: the trichothecene same clan: vomitoxin 3-DON 15-DON nivalenol etc.；
Packing quality proportion of composing is: nano-graphite carbon black 40%, aluminium oxide 40%, Aluminosilicates adsorbent 10%.Silica gel 10%.
Decontaminating column filler configures: filler 2.5g, wherein nano-graphite carbon black 1g, aluminium oxide 1g, Aluminosilicates adsorbent 0.25g.Silica gel 0.25g.
Sampling is pulverized:
Weigh a certain amount of Semen Maydis to pulverize in grinder and point sample,
Cross 20 mesh sieves at ground sample, then weigh 25g pulverizing sample stand-by,
Purified treatment:
The first step, extraction: weigh 25g and pulverize sample, add 100ml acetonitrile/water (v/v:16/84) mixed liquor, shake 2 minutes with high speed homogenization device, use filter paper filtering.
Second step, takes extract 8ml and adds in Multifunctional cleanup column test tube, and then uniform speed slow is pressed downward against decontaminating column so that extract is at the uniform velocity by decontaminating column packing layer, collection and purification solution；
3rd step, takes 4mL and flows through scavenging solution, uses that mycotoxin concentrator is dense to be dried up.
4th step, 1ml flows phased soln concentrate, mixes 1 minute and analyze for HPLC on whirlpool instrument
The analyte response rate: 90～105%, relative standard deviation: less than 5%.
Before and after grain class sample purification, solution collection of illustrative plates refers to Fig. 2.
Application Example 2:(270 column purification)
The trichothecene same clan in grain feed: DON NIV F-X toxin T-2 toxin HT-2 toxin DAS NEO toxin analysis；
Thing to be checked: grain class, such as Semen Tritici aestivi；
Filler configuring condition:
Described packing quality proportion of composing is: nano-graphite carbon black 30%, aluminium oxide 40%, Aluminosilicates adsorbent 20%, silica gel 10%.
Decontaminating column filler configures: filler 3g, wherein nano-graphite carbon black 0.9g, aluminium oxide 1.2g, Aluminosilicates adsorbent 0.6g, silica gel 0.3g.
Sampling is pulverized:
Weigh a certain amount of Semen Maydis to pulverize in grinder and point sample,
Cross 20 mesh sieves at ground sample, then weigh 25g pulverizing sample stand-by
Purified treatment:
The first step, extraction: weigh 25g and pulverize sample, add 100ml acetonitrile/water (v/v:16/84) mixed liquor, shake 2 minutes with high speed homogenization device, use Cao Wen filter paper filtering.
Second step, takes extract 8ml and adds in Multifunctional cleanup column test tube, and then uniform speed slow is pressed downward against decontaminating column so that extract is at the uniform velocity by decontaminating column packing layer, collection and purification solution；
3rd step, takes 4mL and flows through scavenging solution, uses that mycotoxin concentrator is dense to be dried up.
4th step, 1ml flows phased soln concentrate. and mix on whirlpool instrument 1 minute and analyze for HPLC.
The analyte response rate: 82～98%, relative standard deviation: less than 5%.
The method of Application Example 3 (227 post) gas phase
The trichothecene same clan in feedstuff: DON NIV F-X toxin T-2 toxin HT-2 toxin DAS NEO toxin analysis；
Thing to be checked: grain class such as Semen Tritici aestivi；
Filler configuring condition:
Described packing quality proportion of composing is: nano-graphite carbon black 30%, aluminium oxide 40%, Aluminosilicates adsorbent 20%.Silica gel 10%.
Decontaminating column filler configures: filler 3g, wherein nano-graphite carbon black 0.9g, aluminium oxide 1.2g, Aluminosilicates adsorbent 0.6g.Silica gel 0.3g.
Sampling is pulverized:
Weigh a certain amount of Semen Maydis to pulverize in grinder and point sample,
Cross 20 mesh sieves at ground sample, then weigh 25g pulverizing sample stand-by
Purified treatment:
The first step, extraction: weigh 25g and pulverize sample, add 100ml acetonitrile/water (v/v:16/84) mixed liquor, shake 2 minutes with high speed homogenization device, use Cao Wen filter paper filtering；
Second step, takes extract 8ml and adds in Multifunctional cleanup column test tube, and then uniform speed slow is pressed downward against decontaminating column so that extract is at the uniform velocity by decontaminating column packing layer, collection and purification solution；
3rd step, takes 4mL and flows through scavenging solution, uses that mycotoxin concentrator is dense to be dried up；
4th step, 1ml flows phased soln concentrate. and mix on whirlpool instrument 1 minute and analyze for HPLC.
The analyte response rate: 82～98%, relative standard deviation: less than 5%.
Certainly; the present invention can also have other various embodiments; in the case of without departing substantially from present invention spirit and essence thereof; those of ordinary skill in the art can make various corresponding change and deformation according to the present invention, but these change accordingly and deform the protection domain that all should belong to appended claims of the invention.
Claims (2)
1. the nitric acid oxidation processing method of a nano-graphite carbon black, it is characterised in that the method comprises the steps:
(1) 100g nano-graphite carbon black and 500mL nitric acid are taken；
(2) mixed liquor is heated in reflux boiling lasting 8h, obtain aaerosol solution；
(3) by the most static for this suspension placement until solution layering, draw the supernatant and be precipitated layer；
(4) adding the water with supernatant equivalent, ebuillition of heated 1h in the beds of precipitation, obtain suspension, static placement is until solution is layered；
(5) step (3), (4) it are iteratively repeated, the beds of precipitation after repeatedly being washed and the layering solution of the supernatant；
(6) this layering solution carries out in centrifuge washing to separate, until the pH value of the supernatant keeps constant；
(7) being filtered by the layering solution obtained in step (6), the nano-graphite carbon black obtained after filtration is dried in an oven, obtains the nano-graphite carbon black after final nitric acid oxidation processes.
The nitric acid oxidation processing method of nano-graphite carbon black the most according to claim 1, it is characterised in that the mass fraction of nitric acid is 40% in step (1).
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| CN112920900A (en) * | 2019-12-06 | 2021-06-08 | 中国科学院大连化学物理研究所 | Method for preparing zearalenone in chromatographic degreasing |
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| CN102507805A (en) * | 2011-10-27 | 2012-06-20 | 湖南省产商品质量监督检验院 | Method for detecting trichothecene compound in grain and solid phase extraction column for detection |
| CN103801110A (en) * | 2012-11-07 | 2014-05-21 | 江苏维赛科技生物发展有限公司 | Preparation method of deoxynivalenol immunoaffinity column |
| CN104117227A (en) * | 2013-04-28 | 2014-10-29 | 北京华安麦科生物技术有限公司 | Deoxynivalenol immune affinity column and preparation method and use thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102507805A (en) * | 2011-10-27 | 2012-06-20 | 湖南省产商品质量监督检验院 | Method for detecting trichothecene compound in grain and solid phase extraction column for detection |
| CN103801110A (en) * | 2012-11-07 | 2014-05-21 | 江苏维赛科技生物发展有限公司 | Preparation method of deoxynivalenol immunoaffinity column |
| CN104117227A (en) * | 2013-04-28 | 2014-10-29 | 北京华安麦科生物技术有限公司 | Deoxynivalenol immune affinity column and preparation method and use thereof |
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