CN106645451A - Detection method of ochratoxin A in cereals - Google Patents
Detection method of ochratoxin A in cereals Download PDFInfo
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- CN106645451A CN106645451A CN201610879244.0A CN201610879244A CN106645451A CN 106645451 A CN106645451 A CN 106645451A CN 201610879244 A CN201610879244 A CN 201610879244A CN 106645451 A CN106645451 A CN 106645451A
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- ochratoxin
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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
Abstract
The invention discloses a detection method of ochratoxin A in cereals. The detection method comprises steps as follows: a cereal sample is dissolved in an acetonitrile solution, a mixed solution is centrifuged, a supernatant is collected and injected to an amine solid phase extraction column for elution, an eluent is collected and blow-dried, residues are obtained and re-dissolved in a methanol solution, filtering is performed, filtrate is a sample purification liquid, the sample purification liquid is subjected to HPLC-MS-MS (high performance liquid chromatography-tandem mass spectrometry) detection, a detection result is substituted into a curve of a formula 1 for comparison, and the content of ochratoxin A in the sample is obtained. The detection method solves the problem of high cost caused by adoption of an immunoaffinity column for detection of ochratoxin A in the prior art, has the characteristics of being simple, fast, sensitive and accurate, and is applicable to detection of massive samples, and an accurate analysis method can be provided for quality security risk assessment of agricultural products.
Description
Technical field
The present invention relates to agricultural production quality safety detection technique field, relates in particular to ochratoxin A in a kind of cereal
Detection method.
Background technology
Ochratoxin (ochratoxins) is that the one group of structure produced by toxigenic bacterium strains such as aspergillus and Penicilliums is similar
Toxic metabolite material.Ochratoxin includes the similar compound of 7 kinds of structures, wherein with ochratoxin A
(ochratoxinsA, OTA) toxicity is most strong, is distributed most wide.Ochratoxin A is that one kind dissolves in polar organic solvent and dilute carbon
Sour hydrogen sodium solution, is slightly soluble in water, and the chemical name of ochratoxin A is 7- (amino-carbonyl of L- beta-phenyls third)-carboxyl -5- chlorine
Generation -8- hydroxyl -3, the different coumarin (cumarin) of 4- dihydro -3R- methyl, molecular formula is C2OH18ClNO6.Animal toxicity
Test shows that ochratoxin A has immunosupress toxicity, neurotoxicity, teratogenesis and carcinogenicity.1993, international cancer
Ochratoxin A is classified as possible human carcinogen by research center.Therefore countries in the world are paid attention to ochratoxin A
Detection and control, have formulated the limit standard of correlation.State food safety standard of the China in newest promulgation in 2011《In food
Mycotoxin is limited the quantity》The highest Limited Doses for defining ochratoxin A in Grain and its product are 5 μ g/kg.
At present, for the analysis method of ochratoxin A mainly includes liquid chromatography tandem mass spectrometry, high performance liquid chromatography
Method and ELISA.Both at home and abroad for the pre-treating method of ochratoxin A detection in cereal is mainly immune affinity column method,
Because it is selective high, high specificity, sample recovery rate is higher, and the degree of accuracy is high, but has the disadvantage that cost is too high.To evaluate China's cereal
The pollution condition of middle ochratoxin A, it is current to be badly in need of setting up Aspergillus ochraceus in a kind of simple, quick, sensitive, lower-cost cereal
The fast quantitative measurement method for detecting of toxin A.
The content of the invention
It is an object of the invention to：A kind of detection method of ochratoxin A in cereal is provided, the method is：
Extraction and cleaning is first carried out to sample, scavenging solution Jing high performance liquid chromatography tandem mass spectrum technologies (LC/MS/MS) is detected,
The content of ochratoxin A in sample is quantitative determined finally by extraction standard curve.
The method ochratoxin A suitable for detection wheat and corn.
Specifically, a kind of detection method of cereal ochratoxin A of the invention, comprises the steps：
The Liquid Chromatography-Tandem Mass Spectrometry detection method of ochratoxin A, comprises the following steps that in a kind of cereal：
(1) sample cleanup
By acetonitrile and water by volume 4:1 is hybridly prepared into acetonitrile solution, by volume mass ratio (mL/g) 5:1 adds cereal
In sample powder, it is placed in shaking table after 180rpm vibrations 30min, 2500rpm centrifugation 5min collect supernatant；
By 5mL acetonitrile solutions by amino solid-phase extraction column (500ng, 6mL. An Pu companies), leacheate is abandoned；Take on 5mL
Clear liquid crosses amino solid-phase extraction column, abandons post liquid；5mL acetonitrile solutions are taken again and crosses post drip washing twice, abandon leacheate；
By acetonitrile and formic acid by volume 17:3 are configured to chromatogram acetonitrile-formic acid solution, take 10mL acetonitriles-formic acid solution and add
Enter amino solid-phase extraction column, wash-out is enriched in the ochratoxin A on post, collect eluent in clean teat glass, nitrogen
Air-blowing is done；The dissolving of the methyl alcohol of the residue after drying up is taken, (SCAA-104, Town in Shanghai spectrum scientific instrument are limited for 0.22 μm excessively of filter membrane
Company), filtrate is sample cleanup liquid；
(2) the ochratoxin A standard liquid that concentration is followed successively by 0.5,1,5,10,20 μ g/L is taken, efficient liquid is carried out respectively
Phase chromatographic tandem Mass Spectrometer Method, obtains ochratoxin A calibration curve；
(1) (3) carry out high performance liquid chromatography tandem mass spectrum detection, testing result to the sample cleanup liquid that step (1) is obtained
The calibration curve for bringing step (2) acquisition into is compared, with the concentration that external standard method measures Ochratoxin A in sample, according to public
Formula (1) calculates the content of ochratoxin A in sample；
In formula (1)：
X --- Ochratoxin A content in sample, unit be per gram of microgram, μ g/g；
C --- the concentration of Ochratoxin A in prepare liquid, unit is micrograms per millilitre, μ g/mL；
V --- constant volume, unit is milliliter, mL；
M --- sample sample weighting amount, unit for gram, g.
Further, in cereal of the present invention ochratoxin A Liquid Chromatography-Tandem Mass Spectrometry detection method, it is described efficiently
Liquid Chromatography-Tandem Mass Spectrometry detection is specifically referred to：
(1) chromatographic condition：
A) chromatographic column：WatersT-3 chromatographic columns (4.6 × 150mm, 5 μm)；
B) sample size：2μL；
C) column temperature：40℃；
D) flow velocity：0.4mL/min；
E) mobile phase and elution time：
Mobile phase A：The aqueous solution containing 5mmol/L ammonium acetates；
Mobile phase B：Methyl alcohol；
Using linear gradient elution：
90%A, 10%B are initial, and 0-3min, A are 90%-10%, and B is 10%-90%, and 3-5min, A are that 10%, B is
90%；5-7min, A is 10%-90%, and B is 10%-90%；3min is balanced, altogether single sample run time 10min；
(2) Mass Spectrometry Conditions：
Ionization mode is electron spray ionisation positive ion mode (ESI+)；Multiple-reaction monitoring (MRM)；Ion source temperature 500
℃；Residence time 100ms；Atomization air pressure 50psi；Assist gas pressure 50psi；Spray voltage 5500V；Collision cell projects voltage 6V；
Ochratoxin A Mass Spectrometry Conditions parameter is as shown in table 1：
The ochratoxin A Mass Spectrometry Conditions parameter of table 1
Note*：Quota ion.
Further, it is described as described herein in cereal in the Liquid Chromatography-Tandem Mass Spectrometry detection method of ochratoxin A
Cereal is wheat or corn.
Further, it is described as described herein in cereal in the Liquid Chromatography-Tandem Mass Spectrometry detection method of ochratoxin A
Grain sample powder referred to the grain sample powder after 0.5mm hole sizers.
The detection method of Ochratoxin A can be applicable to Aspergillus ochraceus in the cereal such as wheat and corn in a kind of cereal of the present invention
Extraction, purification and the detection of plain A.Compared with other detection methods with it is simple, quick, sensitive and accurate the characteristics of, be applicable to
The detection of batch samples.Simultaneously the present invention solves traditional Ochratoxin A and asks using immune affinity column testing cost is high
Topic.The foundation of this method enables the content Accurate Determining of Ochratoxin A in the cereal such as wheat and corn, can be agricultural product quality
Security risk assessment provides accurate analysis method.
Description of the drawings
Fig. 1 is wheat, corn blank sample chromatography of ions figure.
Fig. 2 is the OTA standard items chromatography of ions figure that concentration is 2g/L.
Fig. 3 is wheat bare substrate calibration curve.
Fig. 4 is corn bare substrate calibration curve.
Fig. 5 is OTA sample chromatogram figures.
Specific embodiment
High performance liquid chromatography tandem mass spectrum used is beautiful for Japanese Shimadzu 20ADXR liquid chromatographic system series connection in embodiment
State's AB3500 mass spectrums.
Embodiment 1 sets up calibration curve
(1) wheat samples bought from market and corn sample are detected by the method for GB/T 25220-2010, is taken
The wheat and corn (as shown in figure 1, wherein Figure 1A is wheat blank sample, Figure 1B is corn blank sample) that OTA is not detected is made
For blank sample；
By acetonitrile and water by volume 4:1 is hybridly prepared into acetonitrile solution, by volume mass ratio (mL/g) 5:1 is separately added into
In blank sample powder (milled 0.5mm hole sizers), after shaking table 180rpm vibration 30min, 2500rpm centrifugation 5min collect supernatant
Liquid；By 5mL acetonitrile solutions by amino solid-phase extraction column (500ng, 6mL. An Pu companies), leacheate is abandoned；Take 5mL supernatant mistakes
Amino solid-phase extraction column, abandoned post liquid；5mL acetonitrile solutions are taken again and crosses post drip washing twice, abandon leacheate；
By acetonitrile and formic acid by volume 17:3 are configured to chromatogram acetonitrile-formic acid solution, take 10mL acetonitriles-formic acid solution and add
Enter amino solid-phase extraction column, wash-out is enriched in the ochratoxin A on post, collect eluent in clean teat glass, nitrogen
Air-blowing is done；The dissolving of the methyl alcohol of the residue after drying up is taken, (SCAA-104, Town in Shanghai spectrum scientific instrument are limited for 0.22 μm excessively of filter membrane
Company), filtrate is sample cleanup liquid (bare substrate)；
(2) take 2g/L Ochratoxin A standard mother liquors (OTA standard items chromatography of ions figure is as shown in Figure 2) and be placed in brown vial
In, with dilution in acetonitrile into the standard reserving solution that concentration is 50 μ g/L；
Respectively with the blank wheat and corn-base dilution above-mentioned standard storing solution in step (1), be made into 0.5 respectively, 1,
5th, the ochratoxin A standard liquid of 10,20 μ g/L, then high performance liquid chromatography tandem mass spectrum detection acquisition standard song is carried out respectively
The bare substrate calibration curve of line, wheat and corn is respectively as shown in Figure 3,4.
Specifically high performance liquid chromatography tandem mass spectrum detection method is：
The μ L of sample size 2,40 DEG C of column temperature.
The condition of high performance liquid chromatography separation is：Chromatographic column is WatersT-3 chromatographic columns (4.6 × 150mm,
5 μm), mobile phase：A is water (ammonium acetate containing 5mmol/L), and B is methyl alcohol, using linear gradient elution：
Elution time：90%A, 10%B are initial, and 0-3min, A are 90%-10%, and B is 10%-90%, and 3-5min, A are
10%, B are 90%；5-7min, A is 10%-90%, and B is 10%-90%；3min is balanced, altogether single sample run time
10min。
Tandem mass spectrum testing conditions are：Electron spray ionisation positive ion mode (ESI+)；Multiple-reaction monitoring (MRM)；Ion gun
500 DEG C of temperature；Residence time 100ms；Atomization air pressure 50psi；Assist gas pressure 50psi；Spray voltage 5500V；Collision cell is projected
Voltage 6V；
Ochratoxin A Mass Spectrometry Conditions parameter is as shown in table 1：
The ochratoxin A Mass Spectrometry Conditions parameter of table 1
Note*：Quota ion.
Ochratoxin A linear equation, detection limit and quantitative limit are as shown in table 2:
The ochratoxin A linear equation of table 2, detection limit and quantitative limit
Calibration curve is set up using matrix mark-on method, in the corresponding range of linearity, Ochratoxin A is in different matrix
It is linear good, coefficient correlation (R) >=0.99.
Sensitivity：The sensitivity of the method assay method that standard solution is diluted with matrix gradient, method it is quantification of
0.5 μ g/L, detection is limited to 0.25 μ g/L.
The rate of recovery：The rate of recovery of method is investigated using matrix mark-on method, high, medium and low (1,2,5 μ g/kg) three
The parallel TIANZHU XINGNAO Capsul scope of concentration 3 is 81.2-102.6%, and relative standard deviation (RSD) is 3.41-4.26%.
Precision：Withinday precision relative standard deviation (RSD) of the Ochratoxin A in wheat and corn-base be
1.71-3.53%, day to day precision relative standard deviation (RSD) is 0.69-1.58%,
Repeatability：Repeated relative standard deviation (RSD) of the Ochratoxin A in wheat and corn-base is 3.72-
4.56%.
The sample detection of embodiment 2
1st, sample cleanup liquid is prepared
The wheat and corn sample of market collection are taken, detection is analyzed by following operating process respectively：
(1) wheat and corn sample are taken, (the size-reduced machine of sample is crushed to can be grinding and sieving by 0.5mm sieves completely
Only), it is placed in 4 DEG C of refrigerators and preserves stand-by；
(2) sample is taken out and is recovered to room temperature, taken 5g sample powders and be placed in 150mL triangular flasks, addition 25mL acetonitriles-
Water 80:The solution of 20 (v/v), after shaking table 180r/min concussion 30min, 2500rpm centrifugation 5min take supernatant；
(3) by 5mL acetonitrile-waters 80:20 (v/v) abandon leacheate by amino solid-phase extraction column；
(4) 5mL supernatants are taken by amino solid-phase extraction column, post liquid was abandoned, 5mL acetonitrile-waters 80 is taken respectively:20(v/v)
Solution cross post drip washing, abandon leacheate；
(5) by chromatogram acetonitrile and formic acid by volume 85:After 15 (v/v) mixing, accurately take 10mL mixed liquors and add amino
Solid-phase extraction column is eluted, and collects whole eluents in clean teat glass, and nitrogen is dried up；
(6) rear residue 1mL methanol solutions dissolving is dried up, after crossing 0.22 μm of filter membrane, filtered fluid treats that sample introduction is analyzed.
(2) sample (corn sample 1, corn sample 2, wheat samples 1, wheat samples 2) to obtaining in the present embodiment is carried
Pure liquid carries out Liquid Chromatography-Tandem Mass Spectrometry detection, as shown in figure 5, wherein, Fig. 5 A are detected OTA sample chromatograms figure for corn sample 1
As a result, Fig. 5 B are the testing result of corn sample 2, and Fig. 5 C are the testing result of wheat samples 1, and Fig. 5 D are the testing result of wheat samples 2；
Bring testing result into calibration curve that embodiment 1 obtains again to compare, the dense of Ochratoxin A in sample is measured with external standard method
Degree, in the content that ochratoxin A in sample is calculated according to formula (1)；
In formula (1)：
X --- Ochratoxin A content in sample, unit be per gram of microgram, μ g/g；
C --- the concentration of Ochratoxin A in prepare liquid, unit is micrograms per millilitre, μ g/mL；
V --- constant volume, unit is milliliter, mL；
M --- sample sample weighting amount, unit for gram, g.
The testing result of ochratoxin A is shown in Table 3 in different samples in the present embodiment:
The testing result of ochratoxin A in the different samples of table 3
| Title concentration (ug/kg) | Corn 1 | Corn 2 | Wheat 1 | Wheat 2 |
| Ochratoxin A | 4.52 | 1.89 | 1.01 | -a |
aLess than detection limit
Meanwhile, for the precision and accuracy of verification method, determine reddish brown in cereal using GB GB/T 25220-2010
Aspertoxin A, content deviation≤5% obtained by the ochratoxin A content obtained by this method and national standard method, it was demonstrated that
Method is accurately and reliably.And the amino solid-phase extraction column price that this method is used is far below the immune affinity column of national standard method, pole
Big saves cost.
Protection scope of the present invention is not limited to description in embodiment, without departing from the modification at the present invention program center
Belong to protection scope of the present invention.
Claims (4)
1. in a kind of cereal ochratoxin A Liquid Chromatography-Tandem Mass Spectrometry detection method, it is characterised in that concrete steps are such as
Under：
(1) sample cleanup
By acetonitrile and water by volume 4:1 is hybridly prepared into acetonitrile solution, and by volume mass 5 are compared:1 adds grain sample powder
In, after 180rpm vibration 30min, 2500rpm centrifugation 5min collect supernatant；Take 5mL supernatants and cross amino solid-phase extraction column, abandon
Cross post liquid；5mL acetonitrile solutions are taken again and crosses post drip washing twice, abandon leacheate；
By acetonitrile and formic acid by volume 17:3 are configured to chromatogram acetonitrile-formic acid solution, take 10mL acetonitriles-formic acid solution and add ammonia
Base solid-phase extraction column, collects eluent and nitrogen is dried up；The dissolving of the methyl alcohol of the residue after drying up is taken, 0.22 μm of filter membrane, filter is crossed
Liquid is sample cleanup liquid；
(2) the ochratoxin A standard liquid that concentration is followed successively by 0.5,1,5,10,20 μ g/L is taken, high-efficient liquid phase color is carried out respectively
Spectrum tandem mass spectrum detection, sets up ochratoxin A calibration curve；
(3) high performance liquid chromatography tandem mass spectrum detection is carried out to the sample cleanup liquid that step (1) is obtained, testing result brings step into
(2) calibration curve for obtaining is compared, and with the concentration that external standard method measures Ochratoxin A in sample, is being calculated according to formula (1)
The content of ochratoxin A in sample；
In formula (1)：
X --- Ochratoxin A content in sample, unit μ g/g；
C --- the concentration of Ochratoxin A in prepare liquid, unit is μ g/mL；
V --- constant volume, unit is mL；
M --- sample sample weighting amount, unit is g.
2. according to claim 1 in cereal ochratoxin A Liquid Chromatography-Tandem Mass Spectrometry detection method, its feature exists
In the high performance liquid chromatography tandem mass spectrum detection is specifically referred to：
(1) chromatographic condition：
A) chromatographic column：WatersT-3 chromatographic columns；
B) sample size：2μL；
C) column temperature：40℃；
D) flow velocity：0.4mL/min；
E) mobile phase and elution time：
Mobile phase A：The aqueous solution containing 5mmol/L ammonium acetates；
Mobile phase B：Methyl alcohol；
Using linear gradient elution：
90%A, 10%B are initial, and 0-3min, A are 90%-10%, and B is 10%-90%, and it is 90% that 3-5min, A are 10%, B；
5-7min, A is 10%-90%, and B is 10%-90%；3min is balanced, altogether single sample run time 10min；
(2) Mass Spectrometry Conditions：
Ionization mode is electron spray ionisation positive ion mode (ESI+)；Multiple-reaction monitoring (MRM)；500 DEG C of ion source temperature；Stay
Stay time 100ms；Atomization air pressure 50psi；Assist gas pressure 50psi；Spray voltage 5500V；Collision cell projects voltage 6V.
3. according to claim 2 in cereal ochratoxin A Liquid Chromatography-Tandem Mass Spectrometry detection method, its feature exists
In the cereal is wheat or corn.
4., according to the Liquid Chromatography-Tandem Mass Spectrometry detection method of ochratoxin A in one of claim 1-3 cereal, it is special
Levy and be, the grain sample powder referred to the grain sample powder after 0.5mm hole sizers.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109001350A (en) * | 2018-06-28 | 2018-12-14 | 山东出入境检验检疫局检验检疫技术中心 | The liquid chromatography-tandem mass spectrometry method of 21 kinds of mycotoxins in Cereals is detected simultaneously |
| CN110187014A (en) * | 2019-03-19 | 2019-08-30 | 东莞理工学院 | A kind of method that LC-MS detects ochratoxin A in food |
| CN114527211A (en) * | 2022-02-18 | 2022-05-24 | 山东省葡萄研究院 | Method for detecting ochratoxin A in grapes by taking graphite powder as purification material |
| CN117491524A (en) * | 2023-11-03 | 2024-02-02 | 粤海永顺泰(广州)麦芽有限公司 | Detection method of cereal cytochalasin E |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109001350A (en) * | 2018-06-28 | 2018-12-14 | 山东出入境检验检疫局检验检疫技术中心 | The liquid chromatography-tandem mass spectrometry method of 21 kinds of mycotoxins in Cereals is detected simultaneously |
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| CN114527211A (en) * | 2022-02-18 | 2022-05-24 | 山东省葡萄研究院 | Method for detecting ochratoxin A in grapes by taking graphite powder as purification material |
| CN114527211B (en) * | 2022-02-18 | 2024-03-15 | 山东省葡萄研究院 | Method for detecting ochratoxin A in grapes by taking graphite powder as purification material |
| CN117491524A (en) * | 2023-11-03 | 2024-02-02 | 粤海永顺泰(广州)麦芽有限公司 | Detection method of cereal cytochalasin E |
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170510 |
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| RJ01 | Rejection of invention patent application after publication |