CN107632079A - A kind of fumonisin special purification post and its application - Google Patents
A kind of fumonisin special purification post and its application Download PDFInfo
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Abstract
The invention discloses a kind of fumonisin special purification post, including column jecket, lower sieve plate, filler and upper sieve plate are sequentially provided with from column jecket outlet end to column jecket liquid feeding end in the column jecket, the particle diameter of the filler is 40~100 μm, filler layering filling, is followed successively by from column jecket outlet end to column jecket liquid feeding end：Florisil silica, polyamino bonded silica gel and amino bonded silica gel, the part by weight of florisil silica, polyamino bonded silica gel and amino bonded silica gel is 1: 1~2: 1~4.The invention also discloses the application of the fumonisin special purification post and the purification method of fumonisin.The filler of the fumonisin special purification post of the present invention has specific adsorption effect to fumonisin, and the special purification post cost is low.
Description
Technical field
The present invention relates to feed and agricultural product quality and safety detection field, more particularly to a kind of fumonisin special purification post
And its application.
Background technology
Fumonisin (Fumonisins, FBs) is one kind by fusarium moniliforme (Fusarium moniliforme), colyliform
Fusariumsp (Fusarium verticillioides), praise sickle-like bacteria (Fusarium proliferatum) and some other more
Water-soluble secondary metabolite caused by fusarium strain.Mainly with FB1、FB2、FB3Form is present, wherein FB1Toxicity is most strong.Volt
Horse toxin has neurotoxicity, pulmonary toxicity, carcinogenicity etc., can cause the white encephalomalacia of horse, pig pulmonary edema syndrome, can also induce
The disease such as human esophagus cancer and Fetal neurotubules malformation.Over nearly 3 years, the investigation in America, Europe and Asia is shown, corn and soybean,
The pollution rate of fumonisin is located at first of mycotoxin in wheat, cereal and Feed Sample, and average pollution rate reaches 64%.According to report
Road, the main feedstuff in China and products thereof second of the three ten-day periods of the hot season horse endotoxin contamination rate is once up to more than 90%, especially with corn and its product
Pollute the most serious, wherein FB1、FB2Recall rate is of a relatively high.
Fumonisin purification method is mainly that the immune affinity column method of purification and strong anion are handed in current existing corn flour
Change column purification method.
Publication No. CN106977600A Chinese patent literature discloses a kind of purification fumonisin B1, aspergillus flavus poison
Element, ochratoxin A, zearalenone immunosorbent and compound affinity column, immunosorbent include solid phase carrier and with
The fumonisin B being coupled on the solid phase carrier1Monoclonal antibody, aflatoxin monoclonal antibody, ochratoxin A monoclonal
Antibody, zearalenone monoclonal antibody.
Fumonisin immune affinity column is expensive, and single branch price greatly improves testing cost at 100 yuan or so.
Strong anion exchange column clean-up effect is not so good as immune affinity column, and cumbersome, and whole purification process at least needs
1h。
Therefore, it is badly in need of a kind of fumonisin special purification post simple to operate, cheap, good purification.
The content of the invention
The present invention provides a kind of fumonisin special purification post, and filler therein has specific adsorption work to fumonisin
With.
A kind of fumonisin special purification post, including column jecket, in the column jecket from column jecket outlet end to column jecket liquid feeding end according to
Secondary to be provided with lower sieve plate, filler and upper sieve plate, the particle diameter of the filler is 40~100 μm, filler layering filling, from column jecket outlet end
It is followed successively by column jecket liquid feeding end：Florisil silica, polyamino bonded silica gel and amino bonded silica gel, florisil silica, polyamino
The part by weight of bonded silica gel and amino bonded silica gel is 1: 1~2: 1~4.
Wherein, florisil silica, polyamino bonded silica gel and amino bonded silica gel be respectively Cleanert Florisil,
Cleanert PSA and Cleanert NH2.Cleanert Florisil are a kind of adsorbents of high selectivity, this adsorbent
Mainly it is made up of three kinds of compositions, silica (84%), magnesia (15.5%) and sodium sulphate (0.5%)；Cleanert NH2
(amino) is the aminopropyl solid phase extraction filler using silica gel as matrix；Cleanert PSA (N- propyl group ethylenediamine) are and NH2Phase
As adsorbent, be the N- propyl group ethylenediamine solid phase extraction fillers using silica gel as matrix.
Three kinds of solid phase extraction fillers carry out layering filling in particular order with specific ratio, have to fumonisin
Specific adsorption acts on, and three's filler is cheap, has wide market promotion prospect.
Preferably, the part by weight of florisil silica, polyamino bonded silica gel and amino bonded silica gel is 1: 2: 2~3.
It is best to the adsorption effect of fumonisin when three kinds of fillers are loaded with aforementioned proportion, fumonisin is returned
Yield is higher.
Preferably, the particle diameter of the florisil silica is 60~100 μm, the particle diameter of the polyamino bonded silica gel is 40
~60 μm, the particle diameter of the amino bonded silica gel is 40~63 μm.
It is further preferred that described upper sieve plate and lower sieve plate are polyethylene sieve plate, its aperture is 0.05~10 μm.
Preferably, the internal diameter of the column jecket is 1~2cm, length is 5~10cm；
The loading of filler is 100~300mg in the column jecket；
The part by weight of florisil silica, polyamino bonded silica gel and amino bonded silica gel is 1: 2: 2~3.
Preferable using suction-operated of the fumonisin special purification post of such scheme to fumonisin, column capacity can meet
Detection demand.
The preparation method of the fumonisin special purification post is：Described lower sieve plate is installed in column jecket outlet end, successively
Florisil silica, polyamino bonded silica gel and amino bonded silica filler are packed into column jecket from column jecket liquid feeding end, then will be upper
Sieve plate is installed in column jecket, is compressed, is produced.
Wherein, upper sieve plate, lower sieve plate and column jecket interference fit are installed.
Present invention also offers a kind of method using above-mentioned fumonisin special purification column purification fumonisin, including with
Lower step：
(1) fumonisin extract solution is flowed through to described fumonisin special purification post；
(2) fumonisin in special purification post is eluted using compounded organic solvent as eluent, after being purified
Fumonisin solution；
The compounded organic solvent is the methanol solution of formic acid or acetic acid.
Preferably, in described compounded organic solvent, the volumetric concentration of formic acid or acetic acid is 1~10%.
In step (2), the elution process of fumonisin is anion exchange procedures, and it is relatively low to add pKa value in eluting solvent
Formic acid or acetic acid can neutralize electric charge on fumonisin, fumonisin is eluted.
It is further preferred that described compounded organic solvent is the methanol solution of formic acid, wherein the volumetric concentration of formic acid is 1
~5%.
The pKa value of formic acid is lower than acetic acid, acid stronger, can more neutralize the electric charge on fumonisin, obtains more preferable
Elution effect.Strong anion exchange column (SAX) is different from, strong anion exchange column is general to elute volt horse with 1% acetic acid methanol
Toxin.
High effective liquid chromatography for measuring is being utilized according to above-mentioned fumonisin special purification post present invention also offers one kind
Application in feed, cereal and/or cereal converted products in fumonisin.
Preferably, described feed includes adding the chicken feed of corn flour, pig feed, ox feed etc.；Described cereal
Including agricultural product such as corn, wheat, sorghum, rice；Described cereal converted products includes the paddy such as corn, wheat, sorghum, rice
Product after thing is processed.
Described fumonisin is fumonisin B1(FB1) and/or fumonisin B2(FB2)。
Preferably, described application comprises the following steps：
(1) feed to be measured, cereal and/or cereal converted products are added into mechanical shaking extraction in Extraction solvent, takes supernatant；
(2) supernatant is flowed through to described fumonisin special purification post；
(3) fumonisin special purification post is eluted with leacheate；
(4) fumonisin in special purification post is eluted with eluent, the fumonisin solution after being purified；
(5) after the fumonisin solution after purification is performed the derivatization, tested and analyzed using high performance liquid chromatography.
In step (1), testing sample is added in extraction solution, 10~60s of vortex oscillation, 1~20min of ultrasonic extraction,
Supernatant is extracted after centrifugation.
The mass volume ratio of testing sample and Extraction solvent is 5g: 15~25ml；
The volume of the supernatant is 1~2ml.
Preferably, described Extraction solvent is the aqueous solution of methanol or acetonitrile；It is further preferred that described extraction is molten
Agent is the methanol aqueous solution that volumetric concentration is 75%.
The impurity of acetonitrile solution extraction is more, and when being detected using high performance liquid chromatography, impurity peaks are to target
The interference at peak is larger, and the impurity of methanol aqueous solution extraction is less and higher to the rate of recovery of fumonisin.
In step (3), described leacheate is methanol, methanol aqueous solution, acetonitrile or acetonitrile solution；Further preferably
, described leacheate is methanol.
In step (4), described eluent is the methanol solution of formic acid or acetic acid, and the volumetric concentration of formic acid or acetic acid is 1
~10%；It is further preferred that described eluent is the formic acid methanol solution that volumetric concentration is 1~10%.
Preferably, described Extraction solvent is the methanol aqueous solution that volumetric concentration is 75%；Described leacheate is first
Alcohol；Described eluent is the formic acid methanol solution that volumetric concentration is 1~10%.
In step (5), the fumonisin solution after purification, which is performed the derivatization, can use prior art.
The fumonisin solution after derivatization is tested and analyzed using high performance liquid chromatography, the mobile phase A of use
For 0.05mol/L citrate buffer solutions (pH 4.0), Mobile phase B is methanol；The gradient elution program used for：0~5min,
70%B~72%B；5~6min, 72%B~75%B；6~11min, 75%B~78%B；11~11.1min, 78%B~
70%B；11.1~15min, 70%B.
Compared with prior art, beneficial effects of the present invention are：
(1) fumonisin special purification column production of the invention is easy, can be mass-produced, also can be by testing staff voluntarily
Filling；
(2) fumonisin special purification post list branch decontaminating column cost of the invention is no more than 4 yuan, equivalent to domestic SAX posts
/ 3rd of price, far below fumonisin immune affinity column (100 yuan /), use cost substantially reduces；
(3) operating procedure is easy, and without activation, loading speed is fast, and whole purification process only needs 6min or so, equivalent to
SAX posts or 1/10th of the immune affinity column clarification time；
(4) after purified, the pigment of extract solution is substantially eliminated, and impurity greatly reduces, good purification, available for liquid phase
With liquid quality detection.
Brief description of the drawings
Fig. 1 is the structural representation of the fumonisin special purification post of the present invention；
Fig. 2 is different fillers to FB1And FB2The block diagram of the rate of recovery；
Fig. 3 is that different proportion mixed fillers are combined to FB1And FB2The block diagram of the rate of recovery；
Fig. 4 is different elution modes to FB1And FB2The block diagram of the rate of recovery；
Fig. 5 is different types of elution to FB1And FB2The block diagram of the rate of recovery；
Fig. 6 is that special purification post compares the clean-up effect of fumonisin figure, and A is without the processing of special purification post, B in figure
To be handled by special purification post.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples.
First, fumonisin special purification post
1st, the selection of filler
Corn flour sample 5g to be measured is weighed into 50mL centrifuge tubes, adds the methanol aqueous solutions of 20mL 75%, vortex oscillation
30s, ultrasonic extraction 10min, 5000rpm centrifugation 5min, takes supernatant 2mL as sample solution.
Choose 8 kinds of solid phase extraction column stuffings, respectively C18, Alu-B, Alu-N, Flo, PSA, PC, NH2, NANO (removes
NANO is 30mg, and remaining filler is 150mg), above-mentioned filler is still in 3h in sample solution, takes supernatant 2mL, nitrogen at 60 DEG C
Air-blowing is done, and is added 0.2mL acetonitrile-aqueous solutions (50: 50, V/V) and is redissolved, and vortex oscillation 1min, ultrasonic 10min, crosses 0.22 μm of filter
Film, efficient liquid phase detection is carried out after derivatization.
As a result find, through PSA, NH2The sample of absorption does not have object substantially, illustrate to fumonisin suction-operated compared with
By force, next to that Flo, PC have a partial adsorbates effect, C18 suction-operated is most weak.
Suction-operated of the filler to fumonisin is further verified by crossing column experiments.8 kinds of fillers are respectively put into and are equipped with
The solid-phase extraction column blank pipe of lower floor's sieve plate, then load sieve plate above filler, it is appropriate to compress.
Sample solution 2mL (applied sample amount is 0.5 μ g), to simplify step, do not elute.The sample liquid eluted with 1% formic acid methanol
The rate of recovery is higher than 1% acetic acid methanol, for example, being equipped with NH2The FB that the solid-phase extraction column of filler is eluted with 1% formic acid methanol1And FB2
Rate of recovery difference 60.86%, 59.70%, and the FB eluted with 1% acetic acid methanol1And FB2Rate of recovery difference 17.62%,
16.97%.Therefore, in follow-up purification condition optimization, eluted with the formic acid methanol of 6mL 1%.
Compare the rate of recovery and clean-up effect of 8 kinds of fillers, as a result see Fig. 2.Flo, PSA and NH in 8 kinds of fillers2The rate of recovery
It is higher, illustrate that this suction-operated of 3 kinds of fillers to fumonisin is stronger.Preferential selection Flo, PSA and NH of the invention2As solid phase
The mixed fillers of extraction column.
2nd, the screening of filler combination ratio
As shown in figure 1, the fumonisin special purification post of the embodiment of the present invention, including column jecket 1, column jecket 1 is interior to be gone out from column jecket
Liquid end to column jecket liquid feeding end is sequentially provided with lower sieve plate 6, filler and upper sieve plate 2.Column jecket internal diameter is 1cm, length 7cm.Sieve plate is
The polyethylene sieve plate in 0.05~10 μm of aperture.Filler layering filling, is followed successively by from column jecket outlet end to column jecket liquid feeding end：Flo、
PSA and NH2。
Flo is florisil silica, and its particle diameter is in 60~100 μ ms；PSA is N- propyl group ethylenediamine bonded silica gels, its
Particle diameter is in 40~60 μ ms；NH2For amino bonded silica gel, its particle diameter is in 40~63 μ ms.
The assemble method of fumonisin special purification post：The sieve plate under the installation of column jecket outlet end, successively by Flo, PSA and
NH2Filler is packed into column jecket from column jecket liquid feeding end, then upper sieve plate is installed in column jecket, is compressed, is produced.
The different filler combinations of fumonisin special purification post are shown in Table 1.
1 different filler combinations of table
Sample solution 2mL is flowed through to the special purification post of above-mentioned 6 kinds of various combinations, eluted with 2mL methanol, then use 2mL
1% formic acid methanol solution elution, be prepared into sample liquid, detected after derivatization using high performance liquid chromatography.As a result figure is seen
3。
The impurity peak area of 6 combinations is more or less the same, and eluent is substantially colorless, and clean-up effect is close.The recovery of combination 5
Rate is of a relatively high, and column capacity can meet detection demand, and prioritizing selection combination 5 is the filler combination of fumonisin special purification post.
2nd, special purification column purification fumonisin is utilized
1st, way choice is eluted
It is that (i.e. filler is 50mg Flo, 50mg PSA and 50mg NH for combination 1 that 2mL sample solutions are flowed through into filler combination2)
Special purification post, eluted respectively from 5 kinds of different elution modes as shown in table 2, control is used as not elute.After elution
Eluted with the formic acid methanol solution that 6ml volumetric concentrations are 1%, collect eluent and be prepared into sample liquid, used after derivatization
High performance liquid chromatography is detected, and as a result sees Fig. 4.
The elution result of the different elution modes of table 2
Appearance features compare：The wash water color not eluted is more deep yellow than the eluent of elution, more muddy, illustrates that elution can
To remove partial pigment, clean-up effect is improved.
Leacheate color containing methanol or acetonitrile is deep yellow, and eluent color compared with sample solution is in colourless, explanation substantially
Eliminate the pigment in sample solution substantially by elution.The leacheate paler colour of 75% methanol aqueous solution, compared with polychrome after elution
Element is stayed on pillar, and wash water color is most deep compared with the eluent of other elution modes, illustrates that 75% methanol aqueous solution elutes
Go depigmentation ability weaker than other solvents.Therefore elution mode of the prioritizing selection containing methanol or acetonitrile.
The rate of recovery compares：FB is not detected in the leacheate of 5 kinds of elution modes1And FB2, illustrate lessivation to FB1And FB2
The rate of recovery do not lose.The eluent rate of recovery of 5 kinds of elution modes is more or less the same, the chromatogram of step elution and the elution of two steps
Impurity peak area is more or less the same, and from the point of view of economical and easy to operate, prioritizing selection methanol is as leacheate.
2nd, the selection of type of elution
It is that (i.e. filler is 50mg Flo, 50mg PSA and 50mg NH for combination 1 that 2mL sample solutions are flowed through into filler combination2)
Decontaminating column, eluted with 2ml methanol, then with 6ml volumetric concentrations be respectively 1%, 2%, 5%, 10% formic acid methanol solution
And volumetric concentration is respectively 1%, 2%, 5%, 10% acetic acid methanol solution, totally 8 kinds of solution are eluted as eluent,
As a result Fig. 5 is seen.
Fumonisin elution process is anion exchange, be can be used in the relatively low eluent of pKa value and on fumonisin
Electric charge.The pKa value of formic acid is lower than acetic acid, acid stronger, can more neutralize the electric charge on fumonisin, and acquisition is preferably washed
It is de-.
The rate of recovery of the formic acid methanol solution elution of various concentrations is more or less the same, and illustrates 1% formic acid methanol solution
Meet the acidity needed for elution.When acetic acid methanol elutes, with the increase of acetic acid concentration, the rate of recovery of fumonisin increases, but second
Sour methanol elution effect is not so good as formic acid methanol all the time.
The rate of recovery and impurity peak area eluted with formic acid methanol solution is above acetic acid methanol solution.From preferentially meeting back
From the point of view of yield, selection volumetric concentration is eluent for 1% formic acid methanol solution.
3rd, the selection of effluent volume
It is that (i.e. filler is 50mg Flo, 50mg PSA and 50mg NH for combination 1 that 2mL sample solutions are flowed through into filler combination2)
Decontaminating column, eluted with 2ml methanol, eluted, the results are shown in Table with 2ml, 4ml, 6ml 1% formic acid methanol solution respectively
3。
The elution result of 3 different effluent volumes of table
As shown in Table 3,2ml eluents can reach the recovery level of 6ml eluents.From saving organic solvent
From the point of view of easy to operate, prioritizing selection 2ml 1% formic acid methanol solution is eluted as eluent.
3rd, fumonisin special purification post is utilizing Feeds by HPLC, cereal and/or cereal processing production
Application in product in fumonisin
1st, application examples：
Comprise the following steps：
(1) sample solution and loading are prepared：Corn flour sample 5g to be measured is weighed into 50mL centrifuge tubes, adds 20mL 75%
Methanol aqueous solution, vortex oscillation 30s, ultrasonic extraction 10min, 5000rpm centrifugation 5min, supernatant 2mL is taken as sample solution, will
It is that (i.e. filler is 25mg Flo, 50mg PSA and 75mg NH for combination 5 that 2ml sample solutions, which flow through filler combination,2) decontaminating column；
(2) elute：Decontaminating column is eluted with 2ml methanol；
(3) elute：Eluted with the formic acid methanol that 2ml volumetric concentrations are 1%, collect eluent；
(4) sample liquid is prepared：By eluent, nitrogen dries up at 60 DEG C, adds 0.2mL acetonitrile-aqueous solutions (50: 50, V/
V) redissolved, vortex oscillation 1min, ultrasonic 10min, be used as sample liquid after crossing 0.22 μm of filter membrane, obtained sample liquid is almost
To be colourless, clean-up effect is preferable；
(5) derivatization：40 μ L samples liquid are taken in 1.5mL centrifuge tubes, add 40 μ L derivatizations solution I (28 μ L β-sulfydryl
Ethanol+8mL 0.1M Boratexes (PH=9.1)) and 40 μ L derivatizations solution IIs (20mg OPA+2mL methanol+6mL
0.1M Boratexes (PH=9.1)), vortex mixed, sample detection in 5min；
(6) sample liquid after derivatization is tested and analyzed using high performance liquid chromatography, analysis condition is as follows：
Chromatographic column is：Agilent HC-C18Analytical (4.6 × 250mm, 5 μm)；
Detection wavelength is：Excitation wavelength 335nm, launch wavelength 440nm；
Mobile phase A is：0.05mol/L citrate buffer solutions (pH4.0), Mobile phase B are methanol；
Gradient elution program：0~5min, 70%B~72%B；5~6min, 72%B~75%B；6~11min, 75%B
~78%B；11~11.1min, 78%B~70%B；11.1~15min, 70%B；
Flow velocity 1.0mL/min；
35 DEG C of column temperature；
The μ L of sample size 50.
Collection of illustrative plates is detected as shown in B in Fig. 6.
2nd, comparative example：
Compared with application examples, the purification by the sample solution of preparation without decontaminating column, directly dried up, redissolved, filtered,
Tested and analyzed after derivatization using high performance liquid chromatography, detection collection of illustrative plates is as shown in A in Fig. 6.After treatment, sample solution
For yellow, wherein containing more pigment.
From fig. 6 it can be seen that not by containing more impurity in the sample of purification column purification, due to doing for impurity
Disturb, FB in its high-efficient liquid phase chromatogram1And FB2Appearance wrapped up by impurity peaks, FB therein can not be detected1And FB2；And pass through
It is less to purify the impurity contained in the sample of column purification, FB1And FB2Appearance it is obvious, without impurity to FB1And FB2Appearance production
Raw interference.
Either apparent or from high-efficient liquid phase chromatogram, decontaminating column all compares the clean-up effect of fumonisin
It is preferable.
Claims (10)
1. a kind of fumonisin special purification post, including column jecket, in the column jecket from column jecket outlet end to column jecket liquid feeding end successively
Provided with lower sieve plate, filler and upper sieve plate, it is characterised in that the particle diameter of the filler is 40~100 μm, filler layering filling, from
Column jecket outlet end to column jecket liquid feeding end is followed successively by：Florisil silica, polyamino bonded silica gel and amino bonded silica gel, Fu Luoli silicon
The part by weight of soil, polyamino bonded silica gel and amino bonded silica gel is 1: 1~2: 1~4.
2. fumonisin special purification post according to claim 1, it is characterised in that the particle diameter of the florisil silica is
60~100 μm, the particle diameter of the polyamino bonded silica gel is 40~60 μm, and the particle diameter of the amino bonded silica gel is 40~63 μ
m。
3. fumonisin special purification post according to claim 2, it is characterised in that described upper sieve plate and lower sieve plate are
Polyethylene sieve plate, its aperture are 0.05~10 μm.
4. the fumonisin special purification post according to any one of claim 2, it is characterised in that
The internal diameter of the column jecket is 1~2cm, and length is 5~10cm；
The loading of filler is 100~300mg in the column jecket；
The part by weight of florisil silica, polyamino bonded silica gel and amino bonded silica gel is 1: 2: 2~3.
5. a kind of method of fumonisin special purification column purification fumonisin using described in any one of Claims 1 to 44, its
It is characterised by, comprises the following steps：
(1) fumonisin extract solution is flowed through to described fumonisin decontaminating column；
(2) fumonisin in decontaminating column is eluted using compounded organic solvent as eluent, the volt horse poison after being purified
Plain solution；
The compounded organic solvent is the methanol solution of formic acid or acetic acid.
6. the method for purification fumonisin according to claim 5, it is characterised in that in described compounded organic solvent,
The volumetric concentration of formic acid or acetic acid is 1~10%.
7. the method for purification fumonisin according to claim 6, it is characterised in that described compounded organic solvent is first
The methanol solution of acid, the wherein volumetric concentration of formic acid are 1~5%.
8. a kind of fumonisin special purification post according to any one of Claims 1 to 4 is utilizing high performance liquid chromatography
Application in measure feed, cereal and/or cereal converted products in fumonisin.
9. application according to claim 8, it is characterised in that comprise the following steps：
(1) feed to be measured, cereal and/or cereal converted products are added into mechanical shaking extraction in Extraction solvent, takes supernatant；
(2) supernatant is flowed through to described fumonisin special purification post；
(3) fumonisin special purification post is eluted with leacheate；
(4) fumonisin in special purification post is eluted with eluent, the fumonisin solution after being purified；
(5) after the fumonisin solution after purification is performed the derivatization, tested and analyzed using high performance liquid chromatography.
10. application according to claim 9, it is characterised in that described Extraction solvent is the first that volumetric concentration is 75%
Alcohol solution；Described leacheate is methanol；Described eluent is the formic acid methanol solution that volumetric concentration is 1~10%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109503393A (en) * | 2018-11-07 | 2019-03-22 | 江苏省农业科学院 | A kind of high speed adverse current chromatogram prepares fumonisin B1The method of standard items |
| CN113000033A (en) * | 2021-02-22 | 2021-06-22 | 中国农业科学院农业质量标准与检测技术研究所 | Amino surface modification purification membrane material and preparation method and application thereof |
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| CN109503393A (en) * | 2018-11-07 | 2019-03-22 | 江苏省农业科学院 | A kind of high speed adverse current chromatogram prepares fumonisin B1The method of standard items |
| CN109503393B (en) * | 2018-11-07 | 2021-10-26 | 江苏省农业科学院 | Preparation of fumonisins B by high-speed countercurrent chromatography1Method for preparing standard substance |
| CN113000033A (en) * | 2021-02-22 | 2021-06-22 | 中国农业科学院农业质量标准与检测技术研究所 | Amino surface modification purification membrane material and preparation method and application thereof |
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| CN107632079B (en) | 2020-05-29 |
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