CN107741462A - A kind of detection method of 16 kinds of mycotoxins - Google Patents
A kind of detection method of 16 kinds of mycotoxins Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8624—Detection of slopes or peaks; baseline correction
- G01N30/8631—Peaks
- G01N30/8634—Peak quality criteria
Abstract
The present invention discloses a kind of detection method of 16 kinds of mycotoxins, its step：Extraction：Precision Sample is weighed in centrifuge tube, adds the extract solution of acetonitrile water acetic acid mixture, vortex or mechanical shaking extraction, then with centrifugation, Aspirate supernatant adds water and the mixing that is vortexed, centrifugation in centrifuge tube, and supernatant crosses teflon membrane filter, collects to obtain filtrate A；Add stable isotope：Accurate filtrate A and the 16 kinds of mycotoxin mixed standard solutions drawn add 14 kinds of mycotoxin stable isotope hybrid working liquid vortexs and mixed in different interpolation pipes respectively.The inventive method is detected using Liquid Chromatography-Tandem Mass Spectrometry instrument, instrumental sensitivity greatly improves, input mode can directly be diluted by sample to be detected, it effectively prevent the loss of object in purification process, reduce the dependence to scavenging material, testing cost is reduced, sample pre-treatments efficiency is improved, realizes multicomponent quickly while detect.
Description
Technical field
The present invention relates to a kind of detection method, the survey of 16 kinds of mycotoxins such as aflatoxin in especially a kind of feed
It is fixed, Liquid Chromatography-Tandem Mass Spectrometry, belong to feed and feedstuff detection field.
Background technology
Mycotoxin is fungi caused poisonous secondary metabolite under optimum conditions, and the mankind, animal can be triggered each
The acute and chronic disease of kind.The mycotoxin species of chief threat human health have Trichothecenes toxoid, volt horse toxoid,
Aspergillus ochraceus toxoid, aspergillus flavus toxoid etc..At present, strict mycotoxin limitation has all been formulated in most countries and regions
Standard, China also pay much attention to mycotoxin contamination problem, are newly revised in 2015《The law of food safety》In, first by biology
Toxin is clearly included in the polluter paid close attention to.Also vomitoxin (DON), zearalenone have been formulated in China
(ZEN), four kinds of aflatoxin B1 (AFB1), ochratoxin (OTA) mycotoxin limit standards, new toxin limitation also exist
Progressively formulate in improving.Due to reasons such as extreme climate and pest and disease damages, the multiple easily hair of Mycotoxins in Cereal, endangers in recent years
Heavy losses are huge.It is reported that there are 31,000,000 tons of feeds and the feedstuff quilt in production, storage, transportation in China every year
Fungal contamination, account for the 6.2% of feed and feedstuff gross annual output amount.In order to ensure China's feed and feedstuff quality peace
Entirely, unnecessary economic loss is avoided, quick monitoring and surveying mycotoxin contamination class, level and its risk are particularly important in time.
Due to mycotoxin wide variety, and collaboration pollution be present, to ensure fungi poison in comprehensive, quick understanding grain
The pollution condition of element, there is an urgent need to a variety of fungies in a kind of simple, quick, sensitive while Accurate Determining feed and feedstuff
The method of toxin.The detection method of mycotoxin mainly has thin-layered chromatography, enzyme linked immunosorbent assay, high performance liquid chromatography at present
Method, liquid chromatography tandem mass spectrometry.Thin-layered chromatography program is complicated, repeatability and repeatability are poor, mutual based on antigen-antibody
Though the enzyme linked immunosorbent assay of effect has higher selectivity, can not accurate quantitative analysis, and easily by matrix interference, produce false sun
Property.High performance liquid chromatography and liquid chromatography tandem mass spectrometry mainly using solid phase extraction column, Mcosep decontaminating columns or are exempted from
Epidemic disease affinity column purifies to sample, although the impurity such as the pigment in extract solution, lipid, albumen can be removed, reduces matrix pair
The influence of toxin Ionization Efficiency, but purification process is numerous and diverse time-consuming, purification cost is high, requires high to operating personnel, and due to true
The chemical property of verticillium toxin is different, polarity scope is wide, can cause the loss of some mycotoxins, influence the accuracy of quantitative result.
Improved with the upgrading of liquid chromatography-mass spectrography, instrumental sensitivity greatly improves, and can directly dilute sample introduction by sample
Mode is detected, and effectively prevent the loss of object in purification process, reduces the dependence to scavenging material, reduce detection into
This, improves sample pre-treatments efficiency, realizes multicomponent quickly while detect.But the ionization process of liquid chromatography-mass spectrometry is easy
Matrix effect can be produced by matrix interference, influences the accurate quantification of toxin.The stable isotope internal standard and target toxin of full carbon markings
Molecular weight is different, but structure, chemical property are identical, and chromatographic retention is also identical with target toxin, while is not present in again
Nature.Therefore the matrix that each mycotoxin can be effectively compensated using scalar quantity in the stable isotope of full carbon markings is imitated
Should, ensure liquid matter precision of analysis and stability.The research of this method is favorably improved feed and the inspection of feedstuff sample
Survey, monitoring efficiency, reduce cost, environmental protection, ensure practitioner's health and safety.This method is formulated subsequent standards, and
Preferable guidance, reference, facilitation are played in the related scientific research of feed and feedstuff pollution aflatoxin, standard formulation.
Therefore, a kind of measure liquid chromatography-tandem matter of 16 kinds of mycotoxins such as aflatoxin in feed is researched and developed
Spectrometry, for the health for developing unpolluted animal husbandry, ensureing the mankind, promote aquaculture sustainable health development, have important
Realistic meaning.
The content of the invention
It is an object of the invention to provide a kind of detection method of 16 kinds of mycotoxins, this method can be easy, quick, accurate
16 kinds of mycotoxins in ground while qualitative and quantitative detection feed and feedstuff, improve feed and feedstuff sample detection, prison
Efficiency is surveyed, cost is reduced, environmental protection, ensures practitioner's health and safety.
The technical scheme is that：A kind of detection method of 16 kinds of mycotoxins, its step：(1) extract：Accurately weigh
0.01g sample 5g is accurate in 50mL centrifuge tubes, adds the extract solution of 20mL acetonitrile-waters-acetic acid mixture, mixed liquor three
Kind liquid volume is than 70:29:1, be vortexed or mechanical shaking extraction 30min, then with 6000r/min centrifuge 10min, draw 0.5mL on
Clear liquid adds 0.5mL water and the mixing that is vortexed in 1.5mL centrifuge tubes, and 10min, supernatant are centrifuged with 12000r/min at 4 DEG C
0.2 μm of teflon membrane filter is crossed, collects to obtain sample filtrate A；(2) stable isotope is added：It is accurate respectively to draw 180uL filters
It is stable to add 14 kinds of mycotoxins of 20uL in different 400uL interpolation pipes for liquid A and 16 kinds of mycotoxin mixed standard solutions
Isotope hybrid working liquid is vortexed after mixing, obtains mixing containing 16 kinds of mycotoxins of target in 14 kinds of mycotoxin stable isotopes
Standardization solution and contain target sample prepare liquid in 14 kinds of mycotoxin stable isotopes；
16 kinds of mycotoxin mixed standard solutions are shown in Table one；
14 kinds of mycotoxin stable isotope hybrid working liquid are shown in Table two；
One 16 kinds of mycotoxin mixed standard solutions of table
2 14 kinds of mycotoxin stable isotope hybrid working liquid concentration of table
(3) will be obtained in upper step containing 16 kinds of mycotoxin hybrid standards of target in 14 kinds of mycotoxin stable isotopes
Solution and it is implanted sequentially liquid chromatography-tandem mass spectrometry system containing target sample prepare liquid in 14 kinds of mycotoxin stable isotopes
System, is detected, that is, obtains final result.
The detection method of 16 kinds of mycotoxins can determine feed and feed simultaneously using Liquid Chromatography-Tandem Mass Spectrometry
Aflatoxin B in raw material1/B2/G1/G2, deoxynivalenol, nivalenol, deoxynivalenol bacterium alkene
Alcohol -3- glucosides, 3- acetyl group deoxynivalenol, 15- acetyl group deoxynivalenol, Gibberella zeae
Ketenes, ochratoxin A, fumonisin B1/B2, T-2/HT-2,16 kinds of mycotoxins of sterigmatocystin.
The detection method of 16 kinds of mycotoxins qualitative, quantitative measure can be raised simultaneously using Liquid Chromatography-Tandem Mass Spectrometry
Aflatoxin B in material and feedstuff1/B2/G1/G2, deoxynivalenol, nivalenol, deoxidation snow it is rotten
Sickle-like bacteria enol -3- glucosides, 3- acetyl group deoxynivalenol, 15- acetyl group deoxynivalenol,
Zearalenone, ochratoxin A, fumonisin B1/B2, T-2/HT-2,16 kinds of mycotoxins of sterigmatocystin；
Qualitative method：With liquid chromatography-mass spectrography condition determination sample, if the chromatographic peak retention time and standard items of detection
Unanimously, it is allowed to which deviation is less than ± 2.5%；The qualitative ion standard working solution suitable with concentration with the relative abundance of quota ion
Relative abundance is consistent, and relative abundance deviation provides no more than table three, then can determine whether measured object in sample be present；
The maximum allowable offset of the qualitative confirmation relative ion abundance of table three
Quantitative determination：With liquid chromatography-mass spectrography condition determination sample, the standard series work containing Isotopic Internal Standard will be prepared
Make solution and be implanted sequentially liquid chromatography-tandem mass instrument from low to high by concentration, after instrument condition is stable, with object
Matter and interior target concentration ratio are that abscissa is set to x-axis), target substance and interior target peak area ratio are that ordinate is set to y-axis, to each
Individual numerical value point carries out least square linear fit, and standard working curve is calculated by formula (1)：
Y=ax+b ... ... ... ... ... (1)
In formula:
Y --- target substance/interior target peak area ratio；
The slope of a --- regression curve；
X --- target substance/interior target concentration ratio；
The intercept of b --- regression curve.
It is containing 16 kinds of mycotoxin mixed standard solutions of target in 14 kinds of mycotoxin stable isotopes and true containing 14 kinds
The response of target sample prepare liquid all should be in instrument linear response range in verticillium toxin stable isotope.
The detection method liquid chromatography tandom mass spectrometry determination of 16 kinds of mycotoxins, using inner mark method ration；16 kinds
The Mass Spectrometry Conditions of mycotoxin, are shown in Table four
The Mass Spectrometry Conditions of 4 16 kinds of mycotoxins of table
Note：Band * is quota ion in table, and for different mass spectrometers, instrument parameter has differences, and joins mass spectrum before measure
Number is optimized to optimal.
The advantage of the invention is that：The inventive method is detected using liquid chromatography-tandem mass spectrometry instrument, instrumental sensitivity
Greatly improve, input mode can be directly diluted by sample and be detected, effectively prevent the loss of object in purification process,
The dependence to scavenging material is reduced, reduces testing cost, sample pre-treatments efficiency is improved, realizes multicomponent quickly while detect.
The stable isotope internal standard of full carbon markings is different from target lps molecule amount, but structure, chemical property are identical, and chromatogram retains
Time is also identical with target toxin, while is not present in nature again.Therefore using demarcation in the stable isotope of full carbon markings
Amount can effectively compensate the matrix effect of each mycotoxin, ensure liquid matter precision of analysis and stability.We
Method is favorably improved feed and feedstuff sample detection, monitoring efficiency, reduces cost, environmental protection, ensures that practitioner is good for
Kang Anquan.This method is formulated subsequent standards, and related scientific research, the standard system of feed and feedstuff pollution aflatoxin
Surely preferable guidance, reference, facilitation are played.
Embodiment
Below by specific embodiment, the invention will be further described, but the present invention is not limited by following examples
It is fixed.
Embodiment 1
The measure Liquid Chromatography-Tandem Mass Spectrometry of 16 kinds of mycotoxins such as aflatoxin in a kind of feed, investigation acetonitrile/
Water/acetic acid (80:19:1 volume ratio) to the extraction efficiency of 16 kinds of toxin.
Embodiment 2
The measure Liquid Chromatography-Tandem Mass Spectrometry of 16 kinds of mycotoxins such as aflatoxin in a kind of feed, investigation acetonitrile/
Water/acetic acid (70:29:1 volume ratio) to the extraction efficiency of 16 kinds of toxin.
Embodiment 3
The measure Liquid Chromatography-Tandem Mass Spectrometry of 16 kinds of mycotoxins such as aflatoxin, matrix effect in a kind of feed
Refer to influence of the component beyond analyte to the Ionization Efficiency of analyte, the endogenous components being mainly derived from sample and
The impurity introduced after sample treatment.Under electro-spray ionization pattern, the mass spectrum response of compound is easily disturbed by matrix,
Influence quantitative detection.This experiment uses the percentage of peak area of the toxin in bare substrate liquid and peak area in the net solution of toxin
To assess matrix effect.Before and after matrix effect and correction matrix effect of 16 kinds of toxin in wheat, corn and paddy extract solution
Rate of recovery result show that aflatoxin etc. has stronger matrix effect in corn and paddy matrix, fumonisin is in paddy
There is stronger matrix effect in matrix, influence the accuracy of result, it is necessary to correct matrix effect to ensure quantitative accuracy.
Embodiment 4
The measure Liquid Chromatography-Tandem Mass Spectrometry of 16 kinds of mycotoxins such as aflatoxin in a kind of feed, in all samples
Stable isotope is added in product and standard liquid, is quantified with toxin peak area with target peak area ratio in corresponding toxin, so as to more
Mending the matrix effect of mycotoxin influences, because DON-3G, 15-AcDON are sold without corresponding stable isotope on the market, therefore
Use respectively similar with its structure, the adjacent 13C-DON of appearance, 13C-3-AcDON is as internal standard.In view of directly extracting 16 kinds
The recovery rate of mycotoxin is very high, and for extraction recovery substantially in 80~120%, Simultaneous Stabilization Isotopic Internal Standard is expensive,
Therefore selection adds stable isotope before upper machine sample introduction.Compared to Isotopic Internal Standard is added before sample extraction, this method is significantly
Reduce the usage amount (being reduced to 20 μ L from 160 μ L) of stable isotope, save testing cost, and can enough effectively compensates
The influence of matrix effect, ensure the accurate of testing result.
Experimental example 1
Investigate acetonitrile/water/acetic acid (80:19:1 volume ratio) and acetonitrile/water/acetic acid (70:29:1 volume ratio) to 16 kinds of poison
The extraction efficiency of element.FB1, FB2 are using acetonitrile/water/acetic acid (80:19:1 volume ratio) extraction when, extraction efficiency is relatively low, recovery
Rate uses acetonitrile between 60-80%:Water:Acetic acid (70:29:1) more than 80%, and other poison can be reached during extract solution
The rate of recovery of element is also between 80%~120%, therefore select acetonitrile:Water:Acetic acid (70:29:1) it is used as sample extracting solution.
Experimental example 2
Investigate stable isotope and matrix effect, matrix effect refer to ionization of the component beyond analyte to analyte
The influence of efficiency, the endogenous components being mainly derived from sample and the impurity introduced after sample treatment.In electro-spray ionization
Under pattern, the mass spectrum response of compound is easily disturbed by matrix, influences quantitative detection.In the stable isotope of full carbon markings
Mark has identical structure, chemical property and chromatogram, mass spectrum behavior with object, therefore matrix effect is also identical, before sample introduction
Target compound caused by stable isotope can compensate for sampling volume, the Ionization Efficiency in ESI sources, ion transmission is added to respond
Fluctuation, ensure that the Stability and veracity of mass spectrometry results.This experiment uses peak face of the toxin in bare substrate liquid
Accumulate with the percentage of peak area in the net solution of toxin to assess matrix effect.16 kinds of toxin are in wheat, corn and paddy extract solution
In matrix effect and correction matrix effect before and after the rate of recovery show aflatoxin etc. have in corn and paddy matrix compared with
Strong matrix effect, fumonisin have stronger matrix effect in paddy matrix, influence the accuracy of result, it is necessary to correct base
Mass effect ensures quantitative accuracy.Therefore, add stable isotope in all samples and standard liquid, with toxin peak area with
Target peak area ratio is quantified in corresponding toxin, is influenceed so as to make up the matrix effect of mycotoxin, due to DON-3G, 15-
AcDON is sold without corresponding stable isotope on the market, therefore uses, appearance adjacent 13C-DON similar with its structure respectively,
13C-3-AcDON is as internal standard.Very high in view of the recovery rate of directly 16 kinds of mycotoxins of extraction, extraction recovery is substantially 80
In~120%, Simultaneous Stabilization Isotopic Internal Standard is expensive, therefore selection adds stable isotope before upper machine sample introduction.Compare
Isotopic Internal Standard is added before sample extraction, the usage amount that this method greatly reduces stable isotope (is reduced to from 160 μ L
20 μ L), testing cost is saved, and can enough effectively compensates the influence of matrix effect, ensures the accurate of testing result.
This method is qualitative and quantitative detection, belongs to feed detection field, can easy, quickly and accurately qualitative, quantitative simultaneously
16 kinds of mycotoxins in feed and feedstuff are detected, the detection to a variety of mycotoxins in feed and feedstuff has positive
Influence, there are broad market prospects.
Claims (4)
1. a kind of detection method of 16 kinds of mycotoxins, its step：
(1) extract：The sample 5g for being accurate to 0.01g accurately is weighed in 50mL centrifuge tubes, is added 20mL acetonitrile-waters-acetic acid and is mixed
The extract solution of liquid is closed, three kinds of liquid volumes of mixed liquor are than 70:29:1, be vortexed or mechanical shaking extraction 30min, then with 6000r/min
Centrifuge 10min, draw 0.5mL supernatants in 1.5mL centrifuge tubes, add 0.5mL water and the mixing that is vortexed, at 4 DEG C with
12000r/min centrifuges 10min, and supernatant crosses 0.2 μm of teflon membrane filter, collects to obtain sample filtrate A；
(2) stable isotope is added：Accurate 180uL filtrates A and the 16 kinds of mycotoxin mixed standard solutions drawn are in difference respectively
400uL interpolation pipes in, add after 14 kinds of mycotoxin stable isotope hybrid working liquid of 20uL are vortexed and mix, contained
16 kinds of mycotoxin mixed standard solutions of target and stablize in 14 kinds of mycotoxin stable isotopes containing 14 kinds of mycotoxins same
Target sample prepare liquid in the element of position；
16 kinds of mycotoxin mixed standard solutions are shown in Table one；
14 kinds of mycotoxin stable isotope hybrid working liquid are shown in Table two；
One 16 kinds of mycotoxin mixed standard solutions of table
2 14 kinds of mycotoxin stable isotope hybrid working liquid concentration of table
(3) will be obtained in upper step containing 16 kinds of mycotoxin mixed standard solutions of target in 14 kinds of mycotoxin stable isotopes
Liquid chromatography-tandem mass spectrometry system is implanted sequentially with containing target sample prepare liquid in 14 kinds of mycotoxin stable isotopes, is entered
Row detection, that is, obtain final result.
A kind of 2. detection method of 16 kinds of mycotoxins according to claim 1, it is characterised in that：This method uses liquid phase color
Spectrum-tandem mass spectrometry can determine aflatoxin B in feed and feedstuff simultaneously1/B2/G1/G2, deoxynivalenol bacterium alkene
Alcohol, nivalenol, deoxynivalenol -3- glucosides, 3- acetyl group deoxynivalenol,
15- acetyl group deoxynivalenol, zearalenone, ochratoxin A, fumonisin B1/B2, it is T-2/HT-2, miscellaneous
16 kinds of mycotoxins of color aspertoxin.
A kind of 3. detection method of 16 kinds of mycotoxins according to claim 1, it is characterised in that：This method uses liquid phase color
Spectrum-tandem mass spectrometry can determine aflatoxin B in feed and feedstuff by qualitative, quantitative simultaneously1/B2/G1/G2, deoxidation snow it is rotten
Sickle-like bacteria enol, nivalenol, deoxynivalenol -3- glucosides, 3- acetyl group deoxynivalenols
Bacterium enol, 15- acetyl group deoxynivalenol, zearalenone, ochratoxin A, fumonisin B1/B2、T-2/
16 kinds of HT-2, sterigmatocystin mycotoxins；
Qualitative method：With liquid chromatography-mass spectrography condition determination sample, if the chromatographic peak retention time of detection and standard items one
Cause, it is allowed to which deviation is less than ± 2.5%；The phase of the qualitative ion standard working solution suitable with concentration with the relative abundance of quota ion
Consistent to abundance, relative abundance deviation provides no more than table three, then can determine whether measured object in sample be present；
The maximum allowable offset of the qualitative confirmation relative ion abundance of table three
Quantitative determination：With liquid chromatography-mass spectrography condition determination sample, by preparing, the standard series work containing Isotopic Internal Standard is molten
Liquid is implanted sequentially liquid chromatography-tandem mass instrument from low to high by concentration, after instrument condition is stable, with target substance and
Interior target concentration ratio is that abscissa is set to x-axis), target substance and interior target peak area ratio are that ordinate is set to y-axis, to each number
Value point carries out least square linear fit, and standard working curve is calculated by formula (1)：
Y=ax+b ... ... ... ... ... (1)
In formula:
Y --- target substance/interior target peak area ratio；
The slope of a --- regression curve；
X --- target substance/interior target concentration ratio；
The intercept of b --- regression curve；
Containing 16 kinds of mycotoxin mixed standard solutions of target in 14 kinds of mycotoxin stable isotopes and contain 14 kinds of fungi poison
The response of target sample prepare liquid all should be in instrument linear response range in plain stable isotope.
4. according to a kind of detection method of 16 kinds of mycotoxins of claim 1 or 3, it is characterised in that：With liquid chromatogram-string
Join mass spectroscopy, using inner mark method ration；The Mass Spectrometry Conditions of 16 kinds of mycotoxins, it is shown in Table the matter of four 4 16 kinds of mycotoxins of table
Spectral condition
。
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| CN108760929A (en) * | 2018-06-13 | 2018-11-06 | 广东省药品检验所（广东省药品质量研究所、广东省口岸药品检验所） | A method of detection 8 kinds of mycotoxins of FRUCTUS CITRI SARCODACTYLIS |
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