CN108593832A - LC-MS-MS methods that are a kind of while measuring six kinds of mycotoxins in corn - Google Patents
LC-MS-MS methods that are a kind of while measuring six kinds of mycotoxins in corn Download PDFInfo
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Abstract
The present invention provides a kind of while measuring the LC MS MS methods of six kinds of mycotoxins in corn, include the following steps：Six kinds of mycotoxins in sample are analyzed to corn with mixed extract and carry out ultrasonic extraction, composite purifying agent purification is added, centrifugation, after membrane filtration, Liquid Chromatography-Tandem Mass Spectrometry detects, standard curve is established using the blank corn sample matrix solution containing six kinds of mycotoxin standard items, matrix matching quantifies standard measure.This method can be with six kinds of main mycotoxins, i.e. DON, FB1, AFB1, T 2, OTA and ZEN in single-time measurement corn；Method quantitative limit is the 1%~4% of national Limited Doses, can meet detection evaluation needs completely；Method precision RSD≤15%, TIANZHU XINGNAO Capsul meet《23,182 2008 feed herbal medicines of GB and other chemical analyte detection testing regulations》Requirement；It compares with national current standard methods, this method is efficient, economic and environment-friendly.
Description
Technical field
The invention belongs to detection technique field, it is related to aflatoxin B1 in corn (AFB1), vomitoxin (DON), T-2
Six kinds of toxin (T-2), ochratoxin A (OTA), zearalenone (ZEN), fumonisin B1 (FB1) main mycotoxins
Assay method more particularly to LC-MS-MS methods that are a kind of while measuring six kinds of mycotoxins in corn.
Background technology
Corn is easy fungal infection as energy feed raw material, because it is rich in carbohydrate (accounting about 72%).Liu
Phoenix sesame etc. (2017) reports 60 corn samples, and aflatoxin B1 pollutes lighter, exceeding standard rate 0 in corn sample, average
Value is 3.0 μ g/kg；Deoxynivalenol pollutes most serious, and exceeding standard rate is up to 70.6%；Zearalenone recall rate is
100%, 535.9 μ g/kg of average value, exceeding standard rate is up to 31.58%.Xie Wenmei etc. (2017) is reported：Three kinds in 81 corn samples
The testing result of toxin is that aflatoxin B1 pollutes relatively light, recall rate 88.89% in corn sample, and average value is
5.03 μ g/kg, exceeding standard rate 0；Zearalenone and vomitoxin recall rate are 100%, the average value difference 78.42 of content
μ g/kg and 846. μ g/kg, exceeding standard rate are respectively 0 and 43.21%.Liu Fengzhi and Xie Wenmei has only surveyed three kinds of poison in corn
Element, corn is also easy in fact infects fumonisin, T-2 toxin and ochratoxin.Li Siyin etc. (2017) reports, 34 parts of corns
In six kinds of mycotoxin testing results, recall rate 26/34, detection has vomitoxin, zearalenone, fumonisin FB1
And OTA.
Currently, China has built up some Mycotoxins in Feed examination criterias, this includes that GB/T 30956-2014 is raised
The measurement (affine in immunity column purification-high performance liquid chromatography) of deoxynivalenol, NY/T 1970-2010 are raised in material
In material in the measurement (liquid matter method) of fumonisin, GB/T 30957-2014 feeds ochratoxin A measurement (affine in immunity
Column purification-high performance liquid chromatography) and NY/T 2071-2011 [21] feed in aflatoxin, zearalenone and T-2
The measurement Liquid Chromatography-Tandem Mass Spectrometry of toxin.It is most in addition to NY/T 2071-2011 can detect three kinds of mycotoxins simultaneously
Standard is single single toxins checking method, and immune affinity column is mostly import, expensive.Existing national standards detection side
Method there are detection efficiencies low, the high disadvantage of testing cost can measure simultaneously in view of this, it is necessary to provide a kind of of low cost
The method of a variety of mycotoxins in corn.
Invention content
The purpose of the present invention is to provide a kind of while measuring the LC-MS-MS methods of six kinds of mycotoxins in corn, the party
Method detection efficiency is high, at low cost, can meet the needs of domestic corn monitoring.
To achieve the above object, the present invention uses following technical scheme：
LC-MS-MS methods that are a kind of while measuring six kinds of mycotoxins in corn comprising following steps：
(1) it extracts
It weighs corn and analyzes sample in centrifuge tube, mixed extract, vortex mixing is added, oscillation carries out ultrasonic extraction；
(2) it purifies
Centrifugal treating is carried out to extracting solution, takes supernatant, composite purifying agent is added and is purified, vortex mixing is stood
Scavenging solution；
(3) it dilutes
It takes scavenging solution to be diluted with water, is vortexed, is filtered after centrifugation, it is to be measured；
(4) preparation of matrix matching standard working solution
Standard mother solution is prepared respectively with the standard items of six kinds of mycotoxins, then mixing deposit is prepared by standard mother solution
Liquid；
Serial different volumes mixing storing solution is drawn in centrifuge tube, nitrogen dries up to obtain mass mixing standard series；
Blank corn sample is taken, scavenging solution is obtained after being handled according to step (1) (2), takes scavenging solution to be added to quality one by one mixed
In standardization series, ultra-pure water dilution is added, step (3) processing is connect, obtains matrix matching standard working solution；
(5) matrix matching sizing technique LC-MS-MS is measured
Step (4) mesostroma matching standard working solution is subjected to LC-MS-MS measurement, according to testing result drawing
Curve；Sample to be tested in step (3) is measured under the same conditions, testing result is compareed with working curve, obtains sample
The content of six kinds of mycotoxins in product liquid, then the content of mycotoxin in sample is calculated.
Mixed extract is acetonitrile, water, formic acid, volume ratio 80 in the step (1)：19：1.
The adding proportion of the mixed extract is to analyze sample per 1g 5mL is added.Preferably, the title sample of the analysis sample
Amount is 8g, and the additive amount of mixed extract is 40mL.
Step (1) the mesoscale eddies mixing time is 15~20s, and duration of oscillation is 10min~20min, when ultrasonic extraction
Between be 30~45min.
Preferably, step (1) the mesoscale eddies mixing time is 20s, duration of oscillation 10min, and the ultrasonic extraction time is
30。
Centrifugation is 5~8min of centrifugation under conditions of 5000~8000r/min in the step (2).
Preferably, centrifugation is to centrifuge 5min under conditions of 8000r/min in the step (2).
The composite purifying agent is epsom salt and C18.Preferably, composite purifying agent additive amount is per 2mL supernatants
180~200mg epsom salts, 110~130mgC18 is added in liquid.It is highly preferred that seven water sulphur of 190mg is added per 2mL supernatants
Sour magnesium, 120mgC18.
Step (2) the mesoscale eddies mixing time is 10~15s, and time of repose is 3~5min.
Step (3) the mesoscale eddies time is 10~15s.
Centrifugation is 5~8min of centrifugation under conditions of 12000~15000r/min in the step (3).
Preferably, centrifugation is to centrifuge 5min under conditions of 15000r/min in the step (3).
It is filtered into the step (3) and is filtered using 0.22 μm of nylon leaching film.
Liquid-phase chromatographic column is ODS columns, specification in the step (5)：3.0μm*150mm.
In the step (5) liquid chromatogram mobile phase A be volume fraction 0.1% aqueous formic acid, Mobile phase B be containing
The methanol solution of 5mM ammonium acetates, 0.1% formic acid of volume fraction.
The eluent gradient elution program of liquid chromatogram is in the step (5)：0-1min, B 5%；3min, B 50%；
8min, B 75%；12min, B 85%；13min, B 90%；14min, B 100%；15min, B 5%；19min, B 5%；
Sample size is 10 μ L, liquid phase flow rate 0.3mL/min.
Mass spectrometry parameters are set as using MRM multiple-reaction monitoring patterns, ESI ion sources, ion source temperature in the step (5)
400 DEG C, 250 DEG C of desolventizing temperature；Desolventizing gas and taper hole gas are N2, Desolvention gas velocity 15L/min；Taper hole gas velocity
3L/min。
Mass spectrum other parameters are as follows in the step (5)：
Compared with prior art, the present invention having the advantages that：
(1) assay method of the invention has selected the mixed extract of specific composition, can be main to six kinds in corn mould
Verticillium toxin carries out onestep extraction, after being purified with composite purifying agent, using liquid chromatogram appropriate and mass spectrometry parameters, is carried out at the same time survey
It is fixed, a globality scheme is formed, realizes while measuring six kinds of main mycotoxins in corn, save detection time, is improved
Detection efficiency；
(2) present invention substitutes existing purification style using self-control compound adsorbent purification, without expensive immune affinity column
Or the Multifunctional cleanup column of other imports, without expensive Isotopic Internal Standard, thus greatly reduce testing cost；
(3) quantitative limit that DON, FB1, AFB1, T-2, OTA and ZEN in corn can be detected in the present invention is followed successively by：200、
22,1,7,3,6 μ g/kg are followed successively by well below national Limited Doses：1000~5000,5000~60000FB1+FB2, 10~30,
500,100,500~1500 μ g/kg；Method precision RSD≤15%, TIANZHU XINGNAO Capsul meet《In GB 23182-2008 feeds
Veterinary drug and other chemical analyte detection testing regulations》Requirement, detectability disclosure satisfy that the needs of domestic monitoring, method efficiently,
It is economic and environment-friendly.
Description of the drawings
Fig. 1 is corn sample total ion current figure；
Fig. 2 is matrix matching standard working solution total ion current figure；
The quota ion and qualitative abundance of ions ratio that Fig. 3 is DON；
The quota ion and qualitative abundance of ions ratio that Fig. 4 is FB1；
The quota ion and qualitative abundance of ions ratio that Fig. 5 is AFB1；
The quota ion and qualitative abundance of ions ratio that Fig. 6 is T-2；
The quota ion and qualitative abundance of ions ratio that Fig. 7 is OTA；
The quota ion and qualitative abundance of ions ratio that Fig. 8 is ZEN；
It is marked in figure as follows：1-don+TIC(+)；2- Huang song toximycin B1TIC (+)；3- fumonisin B1TIC (+)；4-
T-2TIC(+)；5- ochratoxin A TIC (+)；6- zearalenone TIC (-)；7-don+297.00 ＞ 249.20 (+)
CE-11.0；＞ 231.10 8-don+297.00 (+) CE-12.0；＞ 203.10 9-don+297.00 (+) CE-14.0；10- is yellow bent
Toximycin B1 312.90 ＞ 241.00 (+) CE-40.0；Yellow bent 312.90 ＞ 285.05 (+) CE-24.0 of toximycin B1 of 11-；
12- fumonisins B1 722.30 ＞ 352.20 (+) CE-39.0；13- fumonisins B1 722.30 ＞ 334.20 (+) CE-
39.0；＞ 185.10 14-T-2484.20 (+) CE-21.0；15-T-2 484.20 ＞ 215.10 (+) CE-16.0；16- Aspergillus ochraceus
Toxin A 403.90 ＞ 239.00 (+) CE-24.0；17- ochratoxin As 403.90 ＞ 357.95 (+) CE-13.0；18- is beautiful
Zearlenone 317.00 ＞ 131.10 (-) CE29.0；19- zearalenones 317.00 ＞ 175.20 (-) CE24.0.
Specific implementation mode
With reference to specific embodiment, the technical solution that the present invention will be described in detail, so that those skilled in the art can
Understand and implements the present invention.
LC-MS-MS methods that are a kind of while measuring six kinds of mycotoxins in corn comprising following steps：
(1) it extracts
Analysis sample 8.00g is weighed in 50mL centrifuge tubes, mixed extract (acetonitrile is added：Water：Formic acid=80：19：1)
40mL, vortex mixing 20s are placed in ultrasonic extraction 30min in ultrasonic cleaner after vibrating 10min.
(2) it purifies：It takes out, 5min is centrifuged in 8000r/min, draw 2mL supernatants in 15mL centrifuge tubes, be added
190mg epsom salts, 120mgC18, vortex mixing 15s stand 5min.
(3) it dilutes：Aspirate supernatant 0.5mL adds water 0.5mL, vortex 10s, in 15000r/min in 2.5mL centrifuge tubes
5min is centrifuged, 0.22 μm of nylon leaching film is crossed, bottling waits for that machine measures.
(4) preparation of matrix matching standard working solution
With aflatoxin B1 (AFB1), vomitoxin (DON), T-2 toxin (T-2), ochratoxin A (OTA), corn
Zeranol (ZEN), fumonisin B1 (FB1) six kinds of mycotoxins standard items prepare standard mother solution, second of the three ten-day periods of the hot season horse respectively
The solvent of toxin B1 is 50% acetonitrile water, is filled to half bottle, prevents from overflowing after freezing, other mycotoxins are mixed using acetonitrile as solvent
It closes storing solution to be prepared by each standard mother solution, design considerations mycotoxins in feed Limited Doses ratio is prepared, with mother solution in -20 DEG C
It preserves.Mixing Stock concentrations are followed successively by：DON, FB1 and T-2 are 10 μ g/mL, ZEN5 μ g/mL, OTA 0.1 μ g/mL, AFB1
For 0.03 μ g/mL.Mixing storing solution is diluted in 10 times, 20 times, 50 times, 100 times and 200 times 2.5mL centrifuge tubes, nitrogen is blown
Dry (bare substrate to be added) obtains mass mixing standard series.
Blank corn sample is taken, after step (1) and the processing of step (2) method, 0.5mL scavenging solutions is respectively taken, is added to
In the mass mixing standard series of nitrogen drying, 1.00mL, vortex 10s are supplied with ultra-pure water, 5min is centrifuged in 15000r/min,
0.22 μm of nylon leaching film is crossed, matrix matching standard working solution is obtained, bottling waits for that machine measures.
(5) matrix matching sizing technique LC-MS-MS is measured
Step (4) mesostroma matching standard working solution is subjected to LC-MS-MS measurement, according to testing result drawing
Curve；Sample to be tested in step (3) is measured under the same conditions, testing result is compareed with working curve, obtains sample
The content of six kinds of mycotoxins in product liquid, then the content of mycotoxin in sample is calculated.
Wherein chromatographic column is ODS columns, specification：3.0μm*150mm；Mobile phase A is that the formic acid of volume fraction 0.1% is water-soluble
Liquid, Mobile phase B are the methanol solution containing 5mM ammonium acetates, 0.1% formic acid of volume fraction；Eluent gradient elution program is：0-
1min, B 5%；3min, B 50%；8min, B 75%；12min, B 85%；13min, B 90%；14min, B 100%；
15min, B 5%；19min, B 5%；Sample size is 10 μ L, liquid phase flow rate 0.3mL/min.
Mass spectrometry parameters are set as using MRM multiple-reaction monitoring patterns, ESI ion sources, 400 DEG C of ion source temperature, desolventizing
250 DEG C of temperature；Desolventizing gas and taper hole gas are N2, Desolvention gas velocity 15L/min；Taper hole gas velocity 3L/min.Monitor from
The parameters such as son, collision energy, orifice potential are shown in Table 1.
The analytical performance that six kinds of mycotoxins in corn are measured in the present embodiment is shown in Table 2, and the spectrogram measured is shown in Fig. 1-Fig. 8.
1 mass spectrometry parameters of table
Note：The category quota ion that abundance is 100, other is qualitative ion.
Table 2 measures the analytical performance of six kinds of mycotoxins in corn on Shimadzu LC-MS-MS 8050
From table 2 it can be seen that this method can disposably measure six kinds of main mycotoxins in corn, i.e.,：DON、FB1、
AFB1, T-2, OTA and ZEN, method quantitative limit are the 1%~4% of national Limited Doses, can meet detection evaluation needs completely；Side
Method precision RSD≤15%, TIANZHU XINGNAO Capsul meet《GB 23182-2008 feeds herbal medicines and other chemical analyte detection experiments
Regulation》Requirement；It compares with national current standard methods, this method is efficient, economic and environment-friendly.
Above example is only one embodiment of the present of invention, but can not be used as limitation of the present invention, any to be based on
The change and distortion made on the basis of present inventive concept, each falls within protection scope of the present invention, and specific protection domain is to weigh
Subject to sharp claim is recorded.
Claims (10)
1. LC-MS-MS methods that are a kind of while measuring six kinds of mycotoxins in corn, which is characterized in that include the following steps：
(1) it extracts
Analysis sample is weighed in centrifuge tube, mixed extract, vortex mixing is added, oscillation carries out ultrasonic extraction；
(2) it purifies
Centrifugal treating is carried out to extracting solution, takes supernatant, composite purifying agent is added and is purified, vortex mixing stands to obtain purification
Liquid；
(3) it dilutes
It takes scavenging solution to be diluted with water, is vortexed, is filtered after centrifugation, it is to be measured；
(4) preparation of matrix matching standard working solution
With the standard items of six kinds of mycotoxins with standard mother solution processed respectively, then is prepared by standard mother solution and mix storing solution；It inhales
Take serial different volumes mixing storing solution in centrifuge tube, nitrogen dries up to obtain mass mixing standard series；Take blank corn-like
Product obtain scavenging solution after being handled according to step (1) (2), take scavenging solution to be added to one by one in mass mixing standard series, add super
Pure water dilutes, and connects step (3) processing, obtains matrix matching standard working solution；
(5) matrix matching sizing technique LC-MS-MS is measured
Step (4) mesostroma matching standard working solution is subjected to LC-MS-MS measurement, according to testing result drawing curve；
Sample to be tested in step (3) is measured under the same conditions, testing result is compareed with working curve, is obtained in sample liquid
The content of six kinds of mycotoxins, then the content of mycotoxin in sample is calculated.
2. LC-MS-MS methods that are according to claim 1 while measuring six kinds of mycotoxins in corn, which is characterized in that
Mixed extract is acetonitrile, water, formic acid, volume ratio 80 in the step (1)：19：1.
3. LC-MS-MS methods that are according to claim 1 while measuring six kinds of mycotoxins in corn, which is characterized in that
Step (1) the mesoscale eddies mixing time be 15~20s, duration of oscillation be 10~20min, the ultrasonic extraction time be 30~
45min。
4. LC-MS-MS methods that are according to claim 1 while measuring six kinds of mycotoxins in corn, which is characterized in that
Centrifugation is 5~8min of centrifugation under conditions of 5000~8000r/min in the step (2).
5. LC-MS-MS methods that are according to claim 1 while measuring six kinds of mycotoxins in corn, which is characterized in that
The composite purifying agent is epsom salt and C18.
6. LC-MS/MS methods that are according to claim 5 while measuring six kinds of mycotoxins in corn, which is characterized in that
Composite purifying agent additive amount is that 180~200mg epsom salts, 110~130mgC18 is added per 2ml supernatants.
7. LC-MS-MS methods that are according to claim 1 while measuring six kinds of mycotoxins in corn, which is characterized in that
Centrifugation is 5~8min of centrifugation under conditions of 12000~15000r/min in the step (3).
8. LC-MS-MS methods that are according to claim 1 while measuring six kinds of mycotoxins in corn, which is characterized in that
It is filtered into the step (3) and is filtered using 0.22 μm of nylon leaching film.
9. LC-MS-MS methods that are according to claim 1 while measuring six kinds of mycotoxins in corn, which is characterized in that
Liquid chromatogram mobile phase A is the aqueous formic acid of volume fraction 0.1% in the step (5), and Mobile phase B is to contain 5mM acetic acid
The methanol solution of ammonium, 0.1% formic acid of volume fraction；Eluent gradient elution program is：0-1min, B 5%；3min, B 50%；
8min, B 75%；12min, B 85%；13min, B 90%；14min, B 100%；15min, B 5%；19min, B 5%；
Sample size is 10 μ L, liquid phase flow rate 0.3mL/min.
10. LC-MS-MS methods that are according to claim 1 while measuring six kinds of mycotoxins in corn, feature exist
In mass spectrometry parameters are set as using MRM multiple-reaction monitoring patterns, ESI ion sources, ion source temperature 400 in the step (5)
DEG C, 250 DEG C of desolventizing temperature；Desolventizing gas and taper hole gas are N2, Desolvention gas velocity 15L/min；Taper hole gas velocity 3L/
min。
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| CN109900825A (en) * | 2019-03-18 | 2019-06-18 | 黑龙江八一农垦大学 | The method for separating and detecting for the mycotoxin that corn generates in bulk grain container transportational process |
| CN109900825B (en) * | 2019-03-18 | 2022-03-01 | 黑龙江八一农垦大学 | Separation and detection method for mycotoxin generated in transportation process of corn in bulk grain container |
| CN112763599A (en) * | 2020-12-23 | 2021-05-07 | 广东省农业科学院农产品公共监测中心 | Method for detecting zearalenone and ochratoxin A in feed |
| CN114460210A (en) * | 2022-01-29 | 2022-05-10 | 国家粮食和物资储备局科学研究院 | Kit and method for detecting various mycotoxins with high precision |
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