CN104931308A - Method for simultaneously preparing standards of fumonisins B1, B2 and B3 - Google Patents

Method for simultaneously preparing standards of fumonisins B1, B2 and B3 Download PDF

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CN104931308A
CN104931308A CN201510253888.4A CN201510253888A CN104931308A CN 104931308 A CN104931308 A CN 104931308A CN 201510253888 A CN201510253888 A CN 201510253888A CN 104931308 A CN104931308 A CN 104931308A
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fumonisin
phase
standard items
water
preparative chromatography
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CN104931308B (en
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韩铮
赵志辉
郭文博
沈源源
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Shanghai Academy of Agricultural Sciences
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Abstract

The invention provides a method for simultaneously preparing standards of fumonisins B1, B2 and B3. The method comprises the following steps of sample extraction, rough cleaning and medium-pressure preparation. The method for simultaneously preparing the standards of the fumonisins B1, B2 and B3, provided by the invention, is stable and mature, can be suitable for preparing the fumonisins in various cereal matrixes, such as maize, rice, wheat and PDA, and has the advantages that the cost is low, the preparation flow is efficient and rapid, the purity of the standards is high, and the effect is good.

Description

One prepares fumonisin B1 simultaneously, the method for B2 and B3 standard items
Technical field
The present invention relates to agricultural product security detection technique field, relate in particular to one and prepare fumonisin B1 simultaneously, the method for B2 and B3 standard items.
Background technology
Fumonisin is the water-soluble secondary metabolite of being bred generation by fusarium moniliforme (Fusariummoniliforme) under uniform temperature and damp condition, wherein most importantly fumonisin B1, B2 and B3, can extensively pollute the crops such as corn, wheat, rice, there is neurotoxicity, pulmonary toxicity, hepatotoxicity wind agitation, renal toxicity, carcinogenicity, and there is certain immunotoxicity, embryotoxicity and phytotoxicity, bring serious harm to the life and health of people and animals and property safety.
Due to the stronger toxicity of fumonisin and the characteristic of extensively distribution, cause worldwide great attention, carried out the research of the detection technique of fumonisin B1, B2 and B3 at present.Wherein, standard items are important carriers of metering activity especially stoichiometry activity.Development fumonisin standard items, to guaranteeing that the value unification of data, accurate and tractability detect at different levels, all departments, then realize the worldwide authorization of measurement result and provide accurately according to significant for government decision, and it is promoting social development and is promoting also will to play more and more important effect in economic construction.In addition, carry out the research of the aspects such as the examination of fumonisin, formation mechenism, metabolic rule and hazard evaluation, also must use a large amount of fumonisin standard items.
But, Study on Preparation Technology about fumonisin standard items is very weak, existing commercial fumonisin B1, B2 and B3 standard items are primarily of external import, price is very expensive, the wherein price of fumonisin B1 and thousands of every milligram, unit, and fumonisin B3 even reaches nearly ten thousand yuan every milligram.For mouse toxicological experiment the most cheap, if single oral gavage administration 20 milligrams, the cost of once testing and nearly 100,000 yuan, this is obviously not attainable.The costliness of standard items price causes a lot of scientific research to continue.
The bibliographical information of domestic and international existing fumonisin separation and purification is less, mainly carry out roughing out by silica gel column chromatography in conjunction with thin-layered chromatography and centrifugal partition chromatograph method, but these methods all the also exist shortcoming such as single treatment sample size is few, purity is lower, the recovery is not high and preparation efficiency is lower.Therefore, set up a kind of can be used in multiple fumonisin while preparation method's tool be of great significance.
Summary of the invention
The object of the present invention is to provide one to prepare fumonisin B1, the method for B2 and B3 standard items, the method comprises the steps: simultaneously
Sample extraction: first adopted by sample the mixed solution of organic solvent and water to extract;
Solid-Phase Extraction column purification: extract exchanges pre-treatment solid phase pillar through positive ion and slightly purifies;
Middle compacting is standby: be separated with positive preparative chromatography post the standard items preparing fumonisin B1, B2 and B3 respectively by anti-phase.
The purification of the cereal matrix horse second of the three ten-day periods of the hot season toxin B1, B2 and B3 standard items such as the very applicable wheat of the method, corn, rice, PDA.
Specifically:
(1) extracting sample is the grain sample that can be polluted by fumonisin B1, B2 and B3, as corn, wheat, rice, PDA or other grain sample;
(2) extract is the mixed liquor of organic solvent and water, and wherein organic solvent is the similar organic solvent of methyl alcohol, acetonitrile or other character; The ratio of organic solvent and water is: 5/95-95/5 (v/v); The ratio of Extraction solvent and sample is: 0.1/1-100/1 (v/m); Extracting mode is: ultrasonic, concussion, homogeneous or other, extraction time is 10min-4h;
(3) the pre-treatment solid phase pillar for slightly purifying is cation exchange column, and its filler is cation exchange material, as MAX pillar, and the Solid phase cleaned-up post of MultiSep 211Fum pillar or other similar characteristics filler; Flow rate of liquid (comprising sample solution, leacheate, eluent) is 0.1-10mL/min;
(4) in, the standby first step of compacting is reversed-phase preparative chromatography preparation, and the filler of the preparative chromatography post adopted is reverse phase filler, as Unitary C18 preparative chromatography post (10mm × 250mm, 5 μm) or other similar preparative column; Mobile phase A is acetonitrile, methyl alcohol or other organic solvents mutually, and B phase is water or contains formic acid or second aqueous acid, and the ratio of formic acid or acetic acid and water is 0.1%-5% (v/v)), sample size is 0.1-5mL;
(5) in, the standby second step of compacting is the preparation of positive preparative chromatography essence, the filler of the preparative chromatography post adopted is positive phase filling, as Semi-Preparative SB-CN preparative chromatography post (9.4mm × 250mm, 5 μm) or other similar preparative column; Mobile phase A is acetonitrile, methyl alcohol or other organic solvents mutually, and B phase is water or contains formic acid or second aqueous acid, and the ratio of formic acid or acetic acid and water is 0.1%-5% (v/v)), sample size is 0.1-5mL.
Beneficial effect of the present invention is mainly reflected in:
(1) establish first a kind of can simultaneously for the preparation method of fumonisin B1, B2 and B3 tri-kinds of standard items;
(2) compared with existing single fumonisin preparation method, preparation method's efficient quick more of foundation, can obtain fumonisin B1 in 48h, B2 and B3 tri-kinds of each 10mg of standard items;
(3) the fumonisin standard items purity prepared, all higher than 98%, meets experiment needs;
(4) experiment flow is fixed, and repeatable strong, general experimenter's simple training can complete, practical;
(5) preparation cost is cheap, mainly the consumption of instrument, and three kinds of standard items (10mg) consuming cost total prices are less than 2000 yuan.
The preparation method of fumonisin B1, B2 and B3 of the present invention is stable, ripe, and can be applicable to the preparation of the fumonisin in the various types of grain matrix such as corn, rice, wheat, PDA, with low cost, preparation flow efficient quick, standard items purity is high, effective.
Accompanying drawing explanation
Fig. 1 is the LC-MS/MS the qualitative analysis of fumonisin B1, B2 and B3 tri-kinds of standard items that embodiment one prepares, and A is parent ion figure, B is daughter fragment ion figure.
Fig. 2 is fumonisin B1, B2 and B3 tri-kinds of standard items spectrograms that embodiment one prepares
Wherein: (a): the H spectrum of fumonisin B1
(c): the H spectrum of fumonisin B2
(e): the H spectrum of fumonisin B3
(b): the C spectrum of fumonisin B1
(d): the C spectrum of fumonisin B2
(f): the C spectrum of fumonisin B3.
Embodiment
Below in conjunction with specific embodiment, the present invention is further described, but protection scope of the present invention is not limited in this:
Oasis MAX solid-phase extraction column (Waters company, the U.S.)
Unitary C 18preparative chromatography post (Hua Puxinchuan Science and Technology Ltd., China)
Semi-Preparative SB-CN preparative chromatography post (Agilent company, the U.S.)
Thermo C18 chromatographic column (Thermo Fisher company, the U.S.)
Diode array detector (UPLC-PDA) (Waters company, the U.S.) joined by Ultra Performance Liquid Chromatography instrument
The preparation of embodiment one fumonisin B1, B2, B3 standard items
1, sample extraction
The rice sample (random commercially available rice, filters out the sample polluted by fumonisin) polluted by fumonisin after oven dry is put into solids breaker pulverize, by 1mm aperture screen filtration.Get 200 ± 0.01g sample powder and be placed in 2000mL wide-necked bottle, add 1000mL acetonitrile-water (50:50, v/v) solution and put shaking table 150rpm shaken overnight, then with whatma5 Filter paper filtering.Filter cake is resuspended with 1000mL acetonitrile-water (50:50, v/v), and 150rpm vibrates 2h, filters.Merging twice rearmounted Rotary Evaporators of filtrate, 40 DEG C of content being concentrated into acetonitrile in extract is 10% (v/v) left and right.
2, Solid-Phase Extraction column purification
Get 20mL extract and be placed in 50mL centrifuge tube, add 10mL normal hexane, the centrifugal 10min of 3000r/min, abandon supernatant and middle greasy dirt, take off layer solution and cross MAX post.MAX post uses 5mL methyl alcohol and 5mL methanol-water (3:1 successively, v/v) activate, then add 10mL sample liquid, then add 5mL methanol-water (3:1 successively, and 5mL methyl alcohol drip washing MAX pillar v/v), finally use 10mL methanol-acetic acid (99:1, v/v) wash-out, collect eluent, dry up at 40 DEG C of nitrogen, residue acetonitrile-water (50:50, v/v) is settled to 1mL, stand-by after crossing 0.22 μm of filter membrane.
3, middle compacting is standby
3.1Unitary C 18preparative chromatography Column preparation
Chromatographic condition: Unitary C 18preparative chromatography post (10mm × 250mm, 5 μm); Mobile phase A is for containing 0.1% first aqueous acid (v/v), and Mobile phase B is acetonitrile; Flow velocity 3.0mL/min; Sample size 1000 μ L.Elution requirement is arranged in table 1.
Table 1 preparative liquid chromatography condition of gradient elution
3.2Unitary C 18preparative chromatography post cut gathers
Through Unitary C 18preparative chromatography post is separated and makes FB 1, FB 2and FB 3be separated completely, in different time sections, gather FB respectively 1, FB 2and FB 3cut, arranges respectively between different sample and washes pin program, prevent different sample cross contamination.Different sample collection and wash pin set of time as table 2.
Table 2 different fractions is collected and is washed pin set of time
3.3Semi-Preparative SB-CN preparative chromatography Column preparation
Chromatographic condition: Semi-Preparative SB-CN preparative chromatography post (9.4mm × 250mm, 5 μm); Mobile phase is A is acetonitrile, and Mobile phase B is for containing 0.1% first aqueous acid (v/v), and actual conditions is as table 3.
Table 3 Semi-Preparative SB-CN chromatographic column preparation condition
4. freeze drying
FB is contained by what obtain 1, FB 2, FB 3solution under 40 DEG C of conditions rotary evaporation removing organic phase, then be placed in-80 DEG C of preservations further to spend the night rearmounted freeze drier (LL3000 freeze drier, Heto Powerdry company of Denmark) dry, until freeze-drying completely, pressed powder is taken out (preparation efficiency of three kinds of standard items is all more than 60%) ,-20 DEG C of preservations.
Embodiment two
Three kinds of standard items are prepared to embodiment one and carries out qualitative analysis and purity testing
1 liquid chromatography mass combined instrument (LC-MS/MS) qualitative analysis
LC-MS/MS condition: Thermo C18 chromatographic column (2.1mm × 100mm, 5 μm); Mobile phase A is methyl alcohol, and Mobile phase B is for containing 0.1% first aqueous acid (v/v); Gradient elution: 0 ~ 1mim, 50%B ~ 50%B; 1-7min, 50%B ~ 100%B; 7 ~ 8min, 100%B ~ 100%B; 8 ~ 8.2min, 100%B ~ 50%B; 8.2 ~ 9.0min, 50%B ~ 50%B; Flow velocity is 300 μ L/min; Sample size 5 μ L; Column temperature 30 DEG C.Cracked voltage is 1.5V; Spray voltage is 3.5kV; Atomization air pressure adopts electron spray ESI ion gun (negative ions all adopts), scanning forces 3500Pa; Capillary temperature is 350 DEG C; Sheath air pressure 45Pa; Assist gas pressure 15Pa.Sweep limit m/z300 ~ 800; Daughter fragment ion collision voltage is 30eV.
The FB obtained 1, FB 2, FB 3preparation is (ESI under negative ions pattern -and ESI +) carry out full scan, without peak under negative ion, show that gained preparation is not easy negative ionization, then (ESI under positive ion mode +) obtain chromatographic peak that is single, high kurtosis.Qualitative further to characteristic peak, carry out precursor scans in the positive-ion mode, FB 1, FB 2, FB 3the major molecular ion peak of compound as Fig. 1-A, be 722.30 [M+H]+, 706.30 [M+H] +, 706.30 [M+H] +; FB 1, FB 2, FB 3the predominant secondary fragment at major molecular ion peak as Fig. 1-B, at ESI +molecular ion peak 722.30 [M+H] under pattern +predominant secondary fragment be 352.30 [M+H-2TCA-H 2o] +, 334.30 [M+H-2TCA-2H 2o] +with 704.35 [M+H-H 2o] +; Molecular ion peak 706.30 [M+H] +predominant secondary fragment be 354.30 [M+H-2TCA] +, 336.30 [M+H-2TCA-H 2o] +with 318.30 [M+H-2TCA-2H 2o] +; The FB of above data and bibliographical information (Journal of Separation Science, 2010,33:2723 – 2733.) 1, FB 2, FB 3basically identical, authenticating compound is FB 1, FB 2, FB 3.
2 nuclear magnetic resonance qualifications
NMR qualification is a kind of effective means of authenticating compound structure, 1H and the 13C nuclear magnetic spectrum of FB1, FB2, FB3 is as Fig. 2, with bibliographical information (Advances in Experimental medicine and Biology.1996, basically identical 392:75-91), that proof prepares further is highly purified FB1, FB2, FB3.
Diode array detector (UPLC-PDA) full scan joined by 3 Ultra Performance Liquid Chromatography instrument
Under 200nm-400nm condition, full scan is carried out after FB1, FB2, FB3 of preparing being diluted 100 times with acetonitrile-water (50:50, v/v).The mobile phase of UPLC-PDA is: A phase: acetonitrile; B phase: water.Linear gradient elution gradient condition is: 0-7min 10-100%A; 7-8min 100%A; 8-8.1min 100-10%A, 8.1-10min10%A.Flow velocity is 0.3mL/min, and scanning wavelength is 210-400nm.
By UPLC-PDA full scan, purity analysis is carried out to FB1, FB2, FB3 preparation, found that and obtain comparatively pure standard items by Unitary C18 Column preparation, but still there is certain impurity peaks, in contrast, after Semi-Preparative SB-CN preparative column secondary separation purifying, without obvious absorption peaks, highly purified fumonisin can be obtained.
4LC-MS/MS quantified by external standard method measures purity
Accurately take FB1, FB2, FB3 solid 17.168mg, 8.581mg, 6.460mg of preparing respectively in 25mL volumetric flask, be settled to 25mL with acetonitrile-water (50:50, v/v), mixing, then dilutes 10 successively 2, 10 3, 10 4, 10 5doubly, enter LC-MS/MS to measure.LC-MS/MS adopts multiple-reaction monitoring pattern to measure, and monitoring parameter is as shown in table 4.
The mass spectrometry parameters of table 4 FB1, FB2 and FB3
FB1, FB2, FB3 weigh 5 times respectively, to reduce error.Weighing result is as table 5.Then adopt commercial standard items to enter LC-MS/MS as a reference to analyze, detect and obtain the concentration of different extension rate sample and purity as table 6, show that the purity of the fumonisin of preparation is respectively purity 98.760 ± 0.12%, 99.009 ± 0.08%, 98.838 ± 0.65%.
Table 5 FB 1, FB 2and FB 3weighing result
Table 6 difference prepares concentration and the purity of sample
As fully visible, a kind of method simultaneously preparing fumonisin B1, B2 and B3 of the present invention effectively can prepare purifying to fumonisin B1, B2 and B3 in the various types of grain such as corn, wheat, rice, PDA, method is effective and rapid, 3 kinds of each 10mg of mycotoxin standard items can be obtained in 48 hours, and the reappearance of method is high, prepare effective (standard items purity is all higher than 98%).Compared with existing commercial standard items, under the prerequisite ensureing purity, provide cost savings greatly, the research of the various aspects such as follow-up detection, metabolism, toxicity can be promoted.
Protection scope of the present invention is not limited to the description done in embodiment, and the amendment not departing from the present invention program center all belongs to protection scope of the present invention.

Claims (5)

1. prepare a fumonisin B1, the method for B2 and B3 standard items simultaneously, it is characterized in that the method comprises the steps:
Sample extraction: first adopted by sample the mixed solution of organic solvent and water to extract;
Thick purification: extract exchanges pre-treatment solid phase pillar through positive ion and slightly purifies;
Middle compacting is standby: be separated with positive preparative chromatography post the standard items preparing fumonisin B1, B2 and B3 respectively by anti-phase.
2. according to claim 1ly prepare fumonisin B1, the method for B2 and B3 standard items, is characterized in that simultaneously
The mixed liquor of organic solvent and water, wherein organic solvent is methyl alcohol or acetonitrile; The ratio of organic solvent and water is: 5/95-95/5; The ratio of mixed liquor and sample is: 0.1/1-100/1; Extracting mode is: ultrasonic, concussion or homogeneous, extraction time is 10min-4h.
3. according to claim 1ly prepare fumonisin B1, the method for B2 and B3 standard items, is characterized in that simultaneously
Pre-treatment solid phase pillar for slightly purifying is cation exchange column, and its filler is MAX pillar or MultiSep 211 Fum pillar; Flow rate of liquid is 0.1-10mL/min.
4. according to claim 1ly prepare fumonisin B1, the method for B2 and B3 standard items, is characterized in that simultaneously
Time prepared by reversed-phase preparative chromatography, the filler of preparative chromatography post is reverse phase filler, as Unitary C18 preparative chromatography post; Mobile phase A is acetonitrile or methyl alcohol mutually, and B phase is water or contains formic acid or second aqueous acid, and the ratio of formic acid or acetic acid and water is 0.1%-5%, and sample size is 0.1-5mL.
5. according to claim 1ly prepare fumonisin B1, the method for B2 and B3 standard items, is characterized in that simultaneously
During the preparation of positive preparative chromatography essence, the filler of preparative chromatography post is positive phase filling, as Semi-Preparative SB-CN preparative chromatography post, and 9.4mm × 250mm, 5 μm; Mobile phase A is acetonitrile or methyl alcohol mutually, and B phase is water or contains formic acid or second aqueous acid, and the ratio of formic acid or acetic acid and water is 0.1%-5%, and sample size is 0.1-5mL.
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CN107632079A (en) * 2017-08-18 2018-01-26 浙江省农业科学院 A kind of fumonisin special purification post and its application
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CN114875091A (en) * 2022-04-18 2022-08-09 上海市农业科学院 Method for efficiently preparing alternariol
CN115491316A (en) * 2022-07-01 2022-12-20 上海市农业科学院 Preparation method of concealed toxin T-2-3G

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CN107478478A (en) * 2017-08-08 2017-12-15 上海市农业科学院 A kind of fumonisin B1Substrate standard substance and preparation method thereof
CN107632079A (en) * 2017-08-18 2018-01-26 浙江省农业科学院 A kind of fumonisin special purification post and its application
CN107632079B (en) * 2017-08-18 2020-05-29 浙江省农业科学院 Special purifying column for fumonisins and application thereof
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
CN114875091A (en) * 2022-04-18 2022-08-09 上海市农业科学院 Method for efficiently preparing alternariol
CN114875091B (en) * 2022-04-18 2024-01-26 上海市农业科学院 Method for efficiently preparing alternariol
CN115491316A (en) * 2022-07-01 2022-12-20 上海市农业科学院 Preparation method of concealed toxin T-2-3G

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