CN102401820A - Method for detecting content of mycotoxins in wheat - Google Patents
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Abstract
The invention relates to a method for detecting the content of mycotoxins in wheat. The mycotoxins in the wheat are detected by utilizing high performance liquid chromatography-tandem mass spectrometry, and the mycotoxins related to the detection are deoxynivalenol (DON), 3-acetyl (Ac)-DON, 15-Ac-DON, zearalenone (ZEN) and T-2 respectively. The detection method specifically comprises the following steps of: crushing wheat samples by using a crusher, and obtaining coarse extract by using an extracting solution; obtaining a purified toxin extracting solution by using an amino column; preparing mixed toxin standard liquid with different content; detecting each mycotoxin in the toxin extracting solution by adopting the high performance liquid chromatography-tandem mass spectrometry; and obtaining a regression equation of mycotoxin content relative to a peak area according to detection results of the mixed toxin standard liquid, and calculating the content of the DON, the 3-Ac-DON, the 15-Ac-DON, the ZEN and the T-2 in the wheat sample.
Description
Technical field
The invention belongs to the analytical chemistry field, be specifically related to detection method, especially simultaneously to the detection method of DON, 3-Ac-DON, 15-Ac-DON, ZEN, T-2 toxin in the wheat multiple toxin in the wheat.
Background technology
Wheat scab is the important plant disease in China wheat belt, not only causes serious production loss, and because the pathogenic bacteria Fusarium graminearum produces many mycotoxins in cereal, has a strong impact on human and livestock health.This toxoid mainly comprises deoxynivalenol (DON), 3Ac-DON, 15Ac-DON, T-2 and zearalenone (ZEN) etc.The Control Study of China's head blight is gone through many decades; Although all obtaining important achievement aspect agricultural chemicals control and the breeding for disease resistance; But still do not reach ideal control effect; Especially in the Yellow River and Huai He River basin, China wheat main producing region, the wheat breed overwhelming majority is responsive to the head blight performance, and the popular threat of disease is serious.Last decade, based on the parsing to sickle-like bacteria trichothecene family toxin metabolism molecule mechanism, the transgenic breeding of some important toxolysin genes begins to rise, and especially makes substantial progress in U.S. Canada area.
In the biosynthetic metabolism of sickle-like bacteria trichothecene family toxin,
Tri101Acetylation that can catalysis C-3 hydroxyl alleviates the toxicity of synthetic product, is not suppressed by toxin with protection sickle-like bacteria itself.Research shows that the acetylation of C-3 hydroxyl can reduce final synthetic toxin such as DON and T-2 toxicity 100 times.And the final step in the fusarium toxin biosynthesis pathway exactly remove protected C-3 structure, is discharged into outside the thalline with the toxin that is about to have toxicity.
Domestic and international many laboratories from
Fusarium sporotrichoides, Fusarium graminearumIn be separated to
Tri101Gene, and be inserted in the plants such as wheat, paddy rice, tobacco, show toxin resistance preferably.Because
Tri101Come from the toxin producing sickle-like bacteria, and the toxin anabolism is complicated, changes
Tri101Whether dna triticum can become the main body that toxin produces; Perhaps pathogen is after the synthetic main approach Be Controlled of toxin; Whether metabolic bypass can occur, even produce other noxious materials? Consideration in view of to these factors is necessary detection and investigation that the generation and the metabolism situation of the various different toxin in the wheat are carried out system; To guarantee the wheat edible safety, also seem particularly important and set up such detection method.
Present detection method is the characteristic to single toxin in the sample mostly; Adopt the method purification of samples of immune affinity column; The distinct methods of extraction will carry out repeatedly to(for) the multiple toxin in the same sample and different liquid chromatographic detection obtain extract, so could obtain the content of different toxin in the same sample to single toxin.
Summary of the invention
The objective of the invention is to: to the change of route of synthesis in the toxin production process in the wheat; The quantitative detecting method of multiple mycotoxin in the research fast detecting wheat; With the content of guaranteeing in the wheat relevant toxin within limited range, for the edible safety of wheat provides effective guarantee.
The objective of the invention is to realize like this: a kind of detection method to several kinds of mycotoxin levels in the wheat; Be to utilize the method for using high performance liquid chromatography tandem mass spectrum to detect the mycotoxin in the wheat; It is characterized in that: several kinds of mycotoxins that relate in the detection are deoxynivalenol DON, 3-acetyl group-deoxynivalenol 3-Ac-DON, 15-acetyl group-deoxynivalenol 15-Ac-DON, zearalenone ZEN and the T-2 toxin of Fusarium; The toxin titer that adopts is the mixing toxin titer that contains DON, 3-Ac-DON, 15-Ac-DON, ZEN, T-2 toxin, and concrete detection method is:
A) wheat samples is levigate and through 1mm aperture testing sieve with the high speed Universalpulverizer; Take by weighing 10.00 g flours and place 250 mL triangular flasks; The extract that adds 50.0 mL, room temperature shaking table 200 r/min vibration 30 minutes, centrifugal 5 minutes in room temperature 6000 r/min; Collect supernatant, obtain crude extract;
B) nh 2 column is carried out pre-equilibration with the extract of 3 mL, when solvent liquid level arrives nh 2 column adsorbed layer surface, accurately move into 5.0 mL crude extracts immediately, collected the extraction filtrating of nh 2 column with centrifuge tube; Use extract (acetonitrile+water, volume ratio the are 80:20) wash-out of 2 ml again, collect the filtrating of wash-out; Merge the filtrating of extracting filtrating and wash-out, place on the Nitrogen evaporator, bath temperature dries up for 50 ℃; Add eluent then, be settled to 5.0 mL, the toxin extract after being purified;
C) preparation of mixing toxin titer: be configured to 7 kinds of mixing toxin titers that content of toxins is different to the standard items of DON, 3-Ac-DON, 15-Ac-DON, ZEN, T-2 toxin with eluent; Each DON, 3-Ac-DON, 15-Ac-DON, ZEN toxin concentration that mixes in the toxin titer is identical; Be followed successively by 1000 ng/ml, 500 ng/ml, 200 ng/ml, 100 ng/ml, 50 ng/ml, 20 ng/ml and 10 ng/ml from high to low, the concentration of T-2 toxin is followed successively by 50 ng/ml, 25 ng/ml, 10 ng/ml, 5 ng/ml, 2.5 ng/ml, 1.0 ng/ml and 0.5 ng/ml;
D) adopt the method for using high performance liquid chromatography tandem mass spectrum to detect various mycotoxin in the toxin extract;
E) mycotoxin levels is calculated: the testing result according to mixing the toxin titer draws the regression equation of toxin concentration for peak area, calculates the content of DON in the wheat samples, 3-Ac-DON, 15-Ac-DON, ZEN and T-2 toxin.
In the present invention, the nh 2 column in the b step is that Agilent company produces, and specification is 500 mg, 6 mL.
In the present invention, the extract in a and the b step is acetonitrile+water, and their volume ratio is 80:20; Eluent in b and the C step is methyl alcohol+water, and their volume ratio is 20:80.
In the present invention, the testing conditions of using high performance liquid chromatography tandem mass spectrum is in the d step: chromatographic column is SB-C18 post 250 * 4.6 mm, 5 μ m; Moving phase: A:5 mmol/L ammonium acetate solution, B: methyl alcohol, adopt gradient elution, concrete gradient is:
| Time min | Flow velocity mL/min | A% | B% |
| 0 | 0.3 | 80 | 20 |
| 8 | 0.3 | 10 | 90 |
| 13 | 0.3 | 10 | 90 |
| 13.01 | 0.3 | 80 | 20 |
Column temperature: 30 ℃; Sample size: 2 ul; The mass spectrum condition: electric spray ion source holotype, capillary voltage 4 KV, dry gas flow 10 L/min, atomization gas pressure 40 psi adopt the multiple-reaction monitoring type collection, and the mass spectrum acquisition parameter of various different mycotoxins is:
The invention has the advantages that: can measure DON in the wheat, 3Ac-DON, 15-Ac-DON, ZEN, T-2 toxin simultaneously, generally can only detect, have tangible technical advantage to single toxin in the sample with conventional detection.
The invention has the advantages that: remove the impurity in the crude extract with nh 2 column, adopt the extract of acetonitrile+water (volume ratio is 80:20) to extract toxin in the wheat samples, obtain the toxin crude extract, detect the content of multiple toxin in the wheat with the method for liquid matter logotype.
The invention has the advantages that: the moving phase of liquid chromatography makes different toxin to go out the peak in different time through the method for gradient elution, thereby can separate various different toxin effectively.The Mass Spectrometer Method condition is: electric spray ion source (ESI+), capillary voltage 4KV, dry gas flow 10L/min, atomization gas pressure 40 psi, multiple-reaction monitoring (MRM) type collection sample.
The present invention be advantageous in that: content of toxins accurately, reliably in the mensuration wheat.The appearance time of DON is about 3-7 minute, detects to be limited to 10 ng/g; The appearance time of 3-Ac-DON is 7-10 minute, detects to be limited to 10 ng/g; The appearance time of 15-Ac-DON is 7-10 minute, detects to be limited to 10 ng/g; The appearance time of ZEN is 10-13 minute, detects to be limited to 8 ng/g; The appearance time of T-2 toxin is 10-13 minute, detects to be limited to 0.5 ng/g.The detection limit of above toxin all decreases than the single toxins checking method of GB, and sensitivity increases.
Embodiment
Below the wheat that uses of each embodiment be anti-No. 2 wheat samples of life of same batch.
Embodiment 1
Mensuration-immunoaffinity chromatography of deoxynivalenol purifies the content of DON toxin in the high effective liquid chromatography for measuring wheat samples in employing standard GB/T 23503-2009 food.
Wheat samples is levigate and through 1mm aperture testing sieve with the high speed Universalpulverizer, take by weighing 25.00 g samples in 100 mL volumetric flasks, five repetitions are established in experiment; Add 5.0 g polyglycol respectively, water is settled to scale, mixing; Be transferred in the homogeneous cup, high-speed stirred 2 min, quantitative filter paper filters the back and is filtered to clarification with glass fiber filter paper; Collect filtrating, pipette 2 mL filtered fluids and join in the DON toxin immuno-affinity column, pass through immune affinity column with the flow velocity of 1/s; With 5 mLPBS and 5 mL water drip washing successively immune affinity column, until draining pillar;
Add 1.0 mL methanol-eluted fractions pillars, collect eluent, be used for the liquid chromatogram measuring of DON toxin;
Liquid phase chromatogram condition: C18 post (250 * 4.6 mm, 5 μ m), moving phase: methyl alcohol+water (volume ratio is 20:80), flow velocity: 0.8 mL/min, column temperature: 30 ℃, sample size: 50 ul, detect wavelength: 218 nm;
The DON content of toxins calculates: draw the regression equation of toxin concentration for peak area according to the normaltoxin testing result, calculate the content of DON toxin in the wheat samples.
Embodiment 2
Mensuration-immunoaffinity chromatography of T-2 toxin purifies the content of T-2 toxin in the high effective liquid chromatography for measuring wheat samples in employing standard GB/T 23501-2009 food.
Wheat samples is levigate and through 1mm aperture testing sieve with the high speed Universalpulverizer, take by weighing 25.00 g samples in 100 mL volumetric flasks, five repetitions are established in experiment, and use extract: methyl alcohol+water (volume ratio is 80:20) water is settled to scale; Mixing is transferred in the homogeneous cup, high-speed stirred 2 min; Quantitative filter paper filters, and pipettes 10.0 mL and filtrates in 50 mL volumetric flasks, adds water and is settled to scale; Be filtered to clarification with glass fiber filter paper, collect filtrating, measure 10 mL filtered fluids and join in the T-2 toxin immuno-affinity column; Flow velocity with 1/s passes through immune affinity column, with the water wash immune affinity column of 10 mL, until draining pillar;
Add 1.0 mL methanol-eluted fractions pillars, collect eluent, eluent is dried up with nitrogen under 50 ℃; Add 50 μ L 4-dimethylaminopyridine (DMAP) solution and 50 μ L 1-anthracene nitrile (1-AN) solution; Mixing 1 min.50 ℃ of reaction 15 min on turbine mixer, take out the back among cooling 10 min in frozen water, and 50 ℃ of following nitrogen dry up; With 1.0 mL acetonitrile+water (volume ratio is 75:25) dissolving, be used for the liquid chromatogram measuring of T-2 toxin;
Liquid phase chromatogram condition: C18 post (250 * 4.6 mm, 5 μ m), moving phase: acetonitrile+water (volume ratio is 75:25), flow velocity: 1.0 mL/min, column temperature: 30 ℃, sample size: 20 uL, detect wavelength: excitation wavelength 381nm, emission wavelength 470 nm;
The T-2 content of toxins calculates: draw the regression equation of toxin concentration for peak area according to the normaltoxin testing result, calculate the content of T-2 toxin in the wheat samples.
Embodiment 3
Adopt the mensuration-immunoaffinity chromatography of zearalenone in the GB/T 23504-2009 food to purify the content that high performance liquid chromatography detects ZEN toxin in the wheat samples.
Wheat samples is levigate and through 1mm aperture testing sieve with the high speed Universalpulverizer, take by weighing 50.00 g samples in 100 mL volumetric flasks, five repetitions are established in experiment, add 5 g sodium chloride; Use extract: acetonitrile+water (volume ratio is 90:10) is settled to scale, and mixing is transferred in the homogeneous cup; High-speed stirred 2 min, quantitative filter paper filters, and pipettes 10.0 mL and filtrates in 50 mL volumetric flasks; Add water and be settled to scale, be filtered to clarification with glass fiber filter paper behind the mixing, collect filtrating; Measure 10 mL filtered fluids and join in the ZEN toxin immuno-affinity column, use the water wash immune affinity column of 10 mLPBS cleaning buffer solutions and 10 mL successively, until draining pillar;
Add 1.0 mL methanol-eluted fractions pillars, collect eluent, with methanol constant volume to 1 mL;
Liquid phase chromatogram condition: C18 post (250 * 4.6 mm, 5 μ m), moving phase: acetonitrile+water+methyl alcohol (volume ratio is 46:46:8); Flow velocity: 1.0 mL/min, column temperature: 30 ℃, sample size: 20 ul; Detect wavelength: excitation wavelength 274 nm, emission wavelength 440 nm.
The ZEN content of toxins calculates: draw the regression equation of toxin concentration for peak area according to the normaltoxin testing result, calculate the content of ZEN toxin in the wheat samples.
Embodiment 4
Adopt the content of DON, 3-Ac-DON, 15-Ac-DON, ZEN, T-2 toxin in this patent synchronous detection wheat samples.
Wheat samples was pulverized 20 mesh sieves with comminutor; Take by weighing 10.00 g flours and place 250 ml triangular flasks, establish 5 repetitions, add the extract of 50.0 ml acetonitrile+water (volume ratio is 80:20) in each triangular flask respectively; Shaking table 200 r/min vibration 30 minutes; In room temperature 6000 r/min centrifugal 5 minutes, collect supernatant, obtain crude extract;
Nh 2 column (Agilent, 500 mg, 6 ml) is carried out pre-equilibration with the extract (acetonitrile+water, volume ratio are 80:20) of 3 ml; When solvent liquid level arrives nh 2 column adsorbed layer surface, accurately move into 5.0 ml crude extracts immediately, with the extraction filtrating that centrifuge tube was collected nh 2 column, use extract (acetonitrile+water of 2 ml again; Volume ratio is 80:20) wash-out, the filtrating of collecting wash-out merges the filtrating of extracting filtrating and wash-out; Place on the Nitrogen evaporator, bath temperature dries up for 50 ℃, adds eluent (methyl alcohol+water then; Volume ratio is 20:80), be settled to 5.0 ml, the toxin extract after being purified;
The preparation of toxin titer: the standard items of DON, 3-Ac-DON, 15-Ac-DON, ZEN, T-2 with eluent (methyl alcohol+water; Volume ratio is 20:80) dilution; Be made into the standard items of DON, 3-Ac-DON, 15-Ac-DON, ZEN, T-2 toxin with eluent and be configured to 7 mixing toxin titers that content of toxins is different; Each DON, 3-Ac-DON, 15-Ac-DON, ZEN toxin concentration that mixes in the toxin titer is identical; In 7 each mixing toxin titers; The concentration of DON, 3-Ac-DON, 15-Ac-DON, ZEN toxin is followed successively by 1000 ng/ml, 500 ng/ml, 200 ng/ml, 100 ng/ml, 50 ng/ml, 20 ng/ml and 10 ng/ml from high to low, and the concentration of T-2 toxin is followed successively by 50 ng/ml, 25 ng/ml, 10 ng/ml, 5 ng/ml, 2.5 ng/ml, 1.0 ng/ml and 0.5 ng/ml;
Chromatographic condition: SB-C18 post (250 * 4.6 mm, 5 μ m), moving phase: A:5 mmol/L ammonium acetate solution, B: methyl alcohol, adopt gradient elution, concrete gradient is seen table 1, column temperature: 30 ℃, sample size: 2 ul;
Table 1 gradient elution program
The mass spectrum condition: electric spray ion source (ESI+), capillary voltage 4KV, dry gas flow 10 L/min, atomization gas pressure 40 psi, multiple-reaction monitoring (MRM) type collection, the mass spectrum acquisition parameter of various different mycotoxins is seen table 2;
The mass spectrum acquisition parameter of the different mycotoxins of table 2
Mycotoxin levels is calculated: draw the regression equation of toxin concentration for peak area according to the normaltoxin testing result, calculate the content of DON in the wheat, 3-Ac-DON, 15-Ac-DON, ZEN, T-2 toxin respectively.
Embodiment 5
In view of the applicant does not have to find the examination criteria to 3-Ac-DON and 15-Ac-DON toxin at present, therefore do not have to set up detection model to 3-Ac-DON and 15-Ac-DON toxin, in comparison, lack the technical data of independent detection.
The toxin result that table 3 adopts four kinds of distinct methods to detect
Annotate: “ ∕ " expression do not have this result
Visible by table 3, the present invention measure in the wheat content of toxins accurately, reliable.The recovery of the single toxins checking method of the present invention in the GB all between 95%-102%, big-difference too not, and increasing greatly at the detection sensitivity fermentation, DON has improved 50 times than GB sensitivity; T-2 has improved 20 times than GB; ZEN has also improved more than 2 times than GB, and can carry out the detection of 5 kinds of toxin simultaneously, and efficient improves greatly.
Claims (4)
1. the detection method of several kinds of mycotoxin levels in the grow wheat; Be to utilize the method for using high performance liquid chromatography tandem mass spectrum to detect the mycotoxin in the wheat; It is characterized in that: several kinds of mycotoxins that relate in the detection are deoxynivalenol DON, 3-acetyl group-deoxynivalenol 3-Ac-DON, 15-acetyl group-deoxynivalenol 15-Ac-DON, zearalenone ZEN and the T-2 toxin of Fusarium; The toxin titer that adopts is the mixing toxin titer that contains DON, 3-Ac-DON, 15-Ac-DON, ZEN, T-2 toxin, and concrete detection method is:
A) wheat samples is levigate and through 1mm aperture testing sieve with the high speed Universalpulverizer; Take by weighing 10.00 g flours and place 250 mL triangular flasks; The extract that adds 50.0 mL, room temperature shaking table 200 r/min vibration 30 minutes, centrifugal 5 minutes in room temperature 6000 r/min; Collect supernatant, obtain crude extract;
B) nh 2 column is carried out pre-equilibration with the extract of 3 mL, when solvent liquid level arrives nh 2 column adsorbed layer surface, accurately move into 5.0 mL crude extracts immediately, collected the extraction filtrating of nh 2 column with centrifuge tube; Use extract (acetonitrile+water, volume ratio the are 80:20) wash-out of 2 ml again, collect the filtrating of wash-out; Merge the filtrating of extracting filtrating and wash-out, place on the Nitrogen evaporator, bath temperature dries up for 50 ℃; Add eluent then, be settled to 5.0 mL, the toxin extract after being purified;
C) preparation of mixing toxin titer: be configured to 7 kinds of mixing toxin titers that content of toxins is different to the standard items of DON, 3-Ac-DON, 15-Ac-DON, ZEN, T-2 toxin with eluent; Each DON, 3-Ac-DON, 15-Ac-DON, ZEN toxin concentration that mixes in the toxin titer is identical; Be followed successively by 1000 ng/ml, 500 ng/ml, 200 ng/ml, 100 ng/ml, 50 ng/ml, 20 ng/ml and 10 ng/ml from high to low, the concentration of T-2 toxin is followed successively by 50 ng/ml, 25 ng/ml, 10 ng/ml, 5 ng/ml, 2.5 ng/ml, 1.0 ng/ml and 0.5 ng/ml;
D) adopt the method for using high performance liquid chromatography tandem mass spectrum to detect various mycotoxin in the toxin extract;
E) mycotoxin levels is calculated: the testing result according to mixing the toxin titer draws the regression equation of toxin concentration for peak area, calculates the content of DON in the wheat samples, 3-Ac-DON, 15-Ac-DON, ZEN and T-2 toxin.
2. by the detection method of several kinds of mycotoxin levels in the described wheat of claim 1, it is characterized in that: the nh 2 column in the b step is that Agilent company produces, and specification is 500 mg, 6 mL.
3. the detection method of several kinds of mycotoxin levels in the wheat according to claim 1 is characterized in that: the extract in a and the b step is acetonitrile+water, and their volume ratio is 80:20; Eluent in b and the C step is methyl alcohol+water, and their volume ratio is 20:80.
4. the detection method of several kinds of mycotoxin levels in the wheat according to claim 1, it is characterized in that: the testing conditions of using high performance liquid chromatography tandem mass spectrum is in the d step: chromatographic column is SB-C18 post 250 * 4.6 mm, 5 μ m; Moving phase: A:5 mmol/L ammonium acetate solution, B: methyl alcohol, adopt gradient elution, concrete gradient is:
Column temperature: 30 ℃; Sample size: 2 ul; The mass spectrum condition: electric spray ion source holotype, capillary voltage 4 KV, dry gas flow 10 L/min, atomization gas pressure 40 psi adopt the multiple-reaction monitoring type collection, and the mass spectrum acquisition parameter of various different mycotoxins is:
。
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