CN105784860B - The detection method of the aflatoxin of solid sample during a kind of liquor production - Google Patents
The detection method of the aflatoxin of solid sample during a kind of liquor production Download PDFInfo
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Abstract
The invention discloses a kind of detection methods of the aflatoxin of solid sample during liquor production, belong to technical field of food detection.The present invention is respectively detected the presence of aflatoxin in spirit stillage by combined U PLC MS/MS detectors after carrying out related pre-treatment for spirit stillage.It is simple to operate the present invention provides a kind of novel white wine quality safety index detection technique, micro aspergillus flavus poison poison that may be present in spirit stillage timely can be monitored rapidly, to effectively be controlled white wine Quality Safety.
Description
Technical field
The present invention relates to a kind of detection methods of the aflatoxin of solid sample during liquor production, belong to food inspection
Survey technology field.
Background technology
Aflatoxin belongs to mycotoxin, is delimited by the Agency for Research on Cancer of the World Health Organization as " first kind is carcinogenic
Object ".It easily pollutes cereal crops, meat and dairy produce etc., and harmfulness is that being woven with destruction to people and animal's liver group makees
With when serious, liver cancer being caused even dead.
Cereal crops are the main production raw materials of Liquor-making industry, it is more likely that by aflatoxin and the malicious microorganism band of production
Enter in white wine, threatens the safety of liquor production.The safety problem that present food service industry occurs is continuous, and about aflatoxin pair
Liquor production influence report almost without.Therefore, safety research of the verification aflatoxin in liquor production is very
It is necessary.Going from strength to strength with Spirits market simultaneously, by-product lose grain and are also more and more used for feed processing industry, institute
Also to seem particularly significant to the detection for losing aflatoxin in grain.
It is mainly at present corn, paddy, soybean, dairy produce, edible oil, flavouring for the detection object of aflatoxin
Deng；Ferment drinks such as grape wine, and beer also has pertinent literature report；Detection method focuses primarily upon thin-layered chromatography, efficient liquid
Phase chromatography, enzyme-linked immunization, Liquid Chromatography/Mass Spectrometry etc..Since liquor production process is related to plurality of raw materials, multiple-microorganism, and
The generation of a variety of metabolites, so the solid sample during liquor production, such as yeast, fermented grain, vinasse, with cereals etc.
Grain samples are compared, and are extremely complex, and there are a variety of unknown interfering substances in detection process.
However, it is domestic still less for the research of white wine, there is scholar that ELISA method detection yeast, fermented grain is used to lose grain, it is yellow
Water, base liquor, the aflatoxin B1 content in finished wine；Easily there is false positive in ELISA detection methods, and testing result is bigger than normal, and not
The presence that a variety of toxin can be detected simultaneously, for its experimental result, there is still a need for the verifications of accurately qualitative, quantitative.Some scholars use
High performance liquid chromatography detects sorghum, yeast, fermented grain, yellow water, aflatoxin B1 content in finished wine, however this method is deposited
Long between when detecting, the problems such as sensitivity is insufficient, and the type for the aflatoxin that can be detected simultaneously by is few.
Therefore, develop it is a kind of quickly, accurate, high sensitivity, with detecting being sent out for white wine for a variety of aflatoxin simultaneously
The problem of detection method of solid sample during ferment is current urgent need to resolve.
Invention content
In order to overcome the above problem, this method to provide a kind of be based on while UPLC-MS/MS during detection liquor production
The detection method of 4 kinds of aflatoxin of solid sample can quickly and easily realize the solid sample during liquor production,
Such as in vinasse aflatoxin detection.The method of the present invention is easy to operate, time-consuming short, is applicable to batch samples simultaneously
Detection.The method of the present invention is realized to being detected while aflatoxin AFB1, AFB2, AFG1, AFG2, and the rate of recovery is high, steady
It is qualitative preferable.
The detection method of the present invention, includes the following steps：
(1) it pre-processes：Weigh the solid sample after drying, sieving；
(2) it extracts：Certain proportion water and solvent A is added, shakes mixing, obtains mixed liquor；
(3) it saltouts：Salting-out agents, concussion mixing centrifugation are added in mixed liquor；
(4) it purifies：Take the supernatant liquor in step (3) after centrifugation that cleanser, concussion centrifugation is added；
(5) it concentrates：0.22 μm of film is crossed after taking the supernatant liquor after centrifugation in step (4), nitrogen drying to redissolve；
(6) sample introduction is analyzed：Solution example after the middle film excessively of step (5) is subjected to UPLC-MS/MS detections.
In one embodiment of the invention, during the solid sample is spirit stillage or liquor production
Other solid samples, such as yeast, fermented grain.
Specifically, sieving was 20 mesh sieve in the step (1).
Preferably, solvent A is acetonitrile in the step (2).
Preferably, in the step (2), the solid sample addition 10ml water after being dried according to 5g and 15ml acetonitriles.
Preferably, salting-out agents in the step (3) are solid sample addition 1g NaCl and 4g after being dried according to every 5g
MgSO4。
Specifically, concussion mode is concussion up and down manually in the step (3), the concussion time is 1min.
Preferably, cleanser in the step (4), be according to every 5g dry after solid sample addition 150mg PSA and
900mg MgSO4。
Specifically, in the step (4), concussion mode is vortex oscillation, and the concussion time is 30s.
Specifically, centrifugation step in the step (3) and (4), parameter of noncentricity is 4000rpm rotating speeds 5min.
Specifically, in the step (5), nitrogen drying is redissolved in step, and redissolution liquid is mobile phase (mobile phase A and flowing
Phase B by volume 1:1 mixing), volume 0.5mL.
Specifically, UPLC-MS/MS detections solution example amount used is 5 μ L in the step (5).
Preferably, chromatographic condition is using C18 columns in UPLC-MS/MS in the step (6), and mobile phase is A and B, and A is
Formic acid water, B is methanol, using gradient elution.
Preferably, the mobile phase A and B, A mobile phases a concentration of 0.01% (volume fraction), flow velocity 0.500ml/
min。
In one embodiment of the invention, the chromatographic condition is specifically：It is with ACQUITY UPLC BEH C18
Chromatographic column；Using 0.01% formic acid water as mobile phase A phase, using 100% methanol as Mobile phase B phase, flow velocity 0.5ml/min；Elution
Mode is gradient elution, and elution program is as follows：0min, 5% Mobile phase B；7min, 60% Mobile phase B；9min, 100% flowing
Phase B；11.00min 100% Mobile phase B；11.10min 5% Mobile phase B；14.00min 5% Mobile phase B.
Preferably, the Mass Spectrometry Conditions of UPLC-MS/MS are as follows in the step (6)：Ion source is electro-spray ionization source
(ESI)；Spray voltage is 3000V (+)；Ion source temperature is 150 DEG C, and it is 300 DEG C to remove solvent temperature.
Wherein AFB1：Parent ion is 313.10；Qualitative ion is 240.90, collision energy 35V；Quota ion is
268.70 collision energy 32V；AFB2：Parent ion is 315.10；Qualitative ion is 258.90, collision energy 35V；It is quantitative
Ion is 286.90, collision energy 25V；AFG1：Parent ion is 329.10,；Qualitative ion is 242.80, and collision energy is
25V；Quota ion is 310.90, collision energy 20V；AFG2：Parent ion is 331.10；Qualitative ion is 244.90, collision
Energy is 35V；Quota ion is 313.00, collision energy 24V.
In one embodiment of the invention, the method further includes drawing standard song with aflatoxin standard items
Thus line calculates the content of aflatoxin in vinasse sample.
In one embodiment of the invention, the method specifically includes：
(1) it extracts：10g water at low temperature mixings, 15mL acetonitriles is added in 5g distiller's dried grains powder (wet vinasse dried 20 mesh sieve)
Vortex shakes up 30s and is extracted to aspergillus flavus poison poison；
(2) it saltouts：1g NaCl and 4g MgSO are added in mixed liquor4Shake 1min, 4000rpm rotating speeds 5min；It reduces mixed
Closing the water content in extracting solution, saturated aqueous solution promotes mixed liquor to be layered as acetonitrile layer and water layer simultaneously；
(3) it purifies：Step of learning from else's experience (2) saltout after supernatant, scarvenger (150mg PSA, 900mg MgSO is added4) whirlpool
The even 30s of shaking by swirling, 4000rpm rotating speeds 5min；
(4) it concentrates：Step (3) purified supernatant is taken, is redissolved to 1ml methanol after nitrogen drying：0.1% formic acid water
(1:1) in solution, 5 μ L sample introductions UPLC-MS/MS is taken quantitatively to detect after 0.2 μm of membrane filtration.
Beneficial effects of the present invention：
(1) the method for the present invention is to be applied to the detection and analysis of aflatoxin in spirit stillage for the first time.This method is sensitive
Degree is high, simple operation.Pre-treatment is simple to operation time-consuming short, by using Liquid Chromatography/Mass Spectrometry detection time (14min) than having
High performance liquid chromatography detection time (30min) it is shorter；The detection of AFB1 is limited to 0.09 μ g/kg, far below existing white wine sample
The detection limit that product examine is surveyed；A variety of aflatoxin can be detected simultaneously, including：AFB1, AFB2, AFG1, AFG2.
(2) it can be applied to the detection of aflatoxin in other solid samples in vinasse and liquor production system.The present invention
To the progress of spirit stillage sample, sample introduction is analyzed by UPLC-MS/MS for method, detects the content of aflatoxin in spirit stillage,
Analyze speed is fast, while reducing false positive, improves the accuracy of measurement, highly practical.This method is to yellow in spirit stillage
The detection of aspertoxin content has important directive significance, there is guidance to make the timely safety monitoring of liquor production system
With.Advance food security implementation of work in liquor production.
Description of the drawings
Fig. 1 is the separating effect figure of the lower 4 kinds of aflatoxin of chromatographic condition of the present invention.
Specific implementation mode
Experiment material：
Triple level four bars mass spectrographs (waters), the ACOUITY Ultra Performance LC liquid chromatographs (U.S.
Waters companies), ultrapure water machine (Millipore companies of the U.S.), aflatoxin standard items (Sigma companies), acetonitrile, first
Alcohol, formic acid are chromatographically pure, PSA (Shanghai ANPEL Scientific Instrument Co., Ltd.).
Embodiment 1：The qualitative and quantitative detection of aflatoxin in vinasse
It is detected by the following method：
(1) it extracts：10g water at low temperature mixings, 15mL acetonitriles is added in 5g distiller's dried grains powder (wet vinasse dried 20 mesh sieve)
Vortex shakes up 30s and is extracted to aspergillus flavus poison poison；
(2) it saltouts：1g NaCl and 4g MgSO are added in mixed liquor4Shake 1min, 4000rpm rotating speeds 5min；It reduces mixed
Closing the water content in extracting solution, saturated aqueous solution promotes mixed liquor to be layered as acetonitrile layer and water layer simultaneously；
(3) it purifies：Step of learning from else's experience (2) saltout after supernatant, scarvenger (150mg PSA, 900mg MgSO is added4) whirlpool
The even 30s of shaking by swirling, 4000rpm rotating speeds 5min；
(4) it concentrates：Step (3) purified supernatant is taken, is redissolved to 1ml methanol after nitrogen drying：0.1% formic acid water
(1:1) in solution, 5 μ L sample introductions UPLC-MS/MS is gone quantitatively to detect after 0.2 μm of membrane filtration.
The wherein chromatographic condition of UPLC-MS/MS：ACQUITY UPLC BEH C18；Using 0.01% formic acid as mobile phase A
Phase, using 100% methanol as Mobile phase B phase, flow velocity 0.5mL/min；It is eluted by the gradient elution mode of table 1, elutes journey
Sequence is as follows：0min, 5% Mobile phase B；7min, 60% Mobile phase B；9min, 100% Mobile phase B；11.00min 100% flowing
Phase B；11.10min 5% Mobile phase B；14.00min 5% Mobile phase B.Under the chromatographic condition, 4 kinds of aflatoxin can
It is kept completely separate and peak shape is preferable (as shown in Figure 1).
1 eluent gradient of table
The wherein Mass Spectrometry Conditions of UPLC-MS/MS are：Ion source is electro-spray ionization source (ESI)；Spray voltage is
3000V(+)；Ion source temperature is 150 DEG C, and it is 300 DEG C to remove solvent temperature.
Wherein AFB1：Parent ion is 313.10；Qualitative ion is 240.90, collision energy 35V；Quota ion is
268.70 collision energy 32V；AFB2：Parent ion is 315.10；Qualitative ion is 258.90, collision energy 35V；It is quantitative
Ion is 286.90, collision energy 25V；AFG1：Parent ion is 329.10,；Qualitative ion is 242.80, and collision energy is
25V；Quota ion is 310.90, collision energy 20V；AFG2：Parent ion is 331.10；Qualitative ion is 244.90, collision
Energy is 35V；Quota ion is 313.00, collision energy 24V.
It is realized to the Huang in sample through above step by being compared with the appearance time of aflatoxin standard items
The qualitative detection of aspertoxin.In addition, the aflatoxin standard items by using known quantity draw standard curve, by target peak
Area substitutes into standard curve, you can obtains the content of the corresponding aflatoxin in sample introduction sample, and then knows that white wine is given birth to
The content of the aflatoxin in solid sample during production realizes aflatoxin AFB1, AFB2, AFG1, AFG2
Quantitative detection.Other than vinasse sample, yeast, fermented grain sample can also be detected using the method for the present invention.
Embodiment 2：The quantitative detecting method study on the efficiency of the present invention
It is accurate to weigh 5g distiller's dried grains end, be separately added into different volumes standard items mixed solution, according to embodiment 1 method into
Row detection, makes respective standard curve, and specific concentration is shown in Table 2 to table 5.
2 AFB1 standard curve concentration of table
3 AFB2 standard curve concentration of table
4 AFG1 standard curve concentration of table
Table 5AFG2 standard curve concentration
Precision draws above-mentioned each 5ul of serial solution standard solution, and sample introduction is analyzed, records each component chromatographic peak area to be measured,
With a concentration of abscissa of sample introduction (X), peak area is ordinate (Y), carries out regression analysis, as a result (is shown in Table 6) and shows each component lines
Sexual intercourse is good.
6 aflatoxin B1 of table, B2, G1, G2 regression equation and related coefficient
Meanwhile the detection limit of the method for the present invention, quantitative limit, the rate of recovery, stability data are as shown in table 7 to table 10.In addition to
Outside vinasse sample, yeast, fermented grain sample are detected using the method for the present invention, standard curve linear dependence is also fine, inspection
Rising limit, quantitative limit, the rate of recovery and stability are also similar with vinasse sample.
7 aflatoxin B1 of table, B2, G1, G2 detection limit parameter values
8 aflatoxin B1 of table, B2, G1, G2 quantitative limit parameter values
9 aflatoxin B1 of table, B2, G1, G2 rate of recovery experiment parameter values
10 aflatoxin B1 of table, B2, G1, G2 stability (RSD) parameter value
Embodiment 3：Influence of the testing conditions to testing result
The present invention also compares influence of the different disposal method to detection result.
(1) influence of sample state：Wet vinasse are used to replace dry crushing vinasse as sample, other steps are consistent with embodiment 1.
The results show that the content of the aflatoxin eventually detected reduces about 35% than embodiment 1, the stability of detection and recycling
Rate, which receives, to be seriously affected, and cannot achieve effective detection to aflatoxin at all.
(2) influence of Extraction solvent：Methanol is used to replace acetonitrile as Extraction solvent, other steps are consistent with embodiment 1.Knot
Fruit shows that the content of the aflatoxin eventually detected reduces about 22% than embodiment 1, the stability and the rate of recovery of detection
It receives and seriously affects.In addition, inventor also found, acetonitrile, the Huang eventually detected are directly used when being not added with water in Extraction solvent
The content of aspertoxin illustrates that using acetonitrile and water to combine is used as extraction molten than using the combination of acetonitrile and water to reduce about 60%
Agent can significantly improve the accuracy of detection.
(3) influence purified：The purified treatment in 1 step of embodiment (3) is omitted, as a result, it has been found that the Huang eventually detected is bent
The content of mould toxin reduces about 43% than embodiment 1, and the stability and the rate of recovery of detection, which receive, to be seriously affected.This also illustrates this
The purifying treatment method of invention can significantly improve the accuracy of detection.
(4) influence of liquid phase process：Using liquid phase gradient elution program：0min, 5% Mobile phase B；0.10min, 5% stream
Dynamic phase B；6min, 60% Mobile phase B；9min, 100% Mobile phase B；10min, 100% Mobile phase B；10.10min 5% flowing
Phase B；11min, 5% Mobile phase B；The aflatoxin of four types cannot be kept completely separate by the peak shape presented in collection of illustrative plates.
Although the present invention has been described by way of example and in terms of the preferred embodiments, it is not limited to the present invention, any to be familiar with this skill
The people of art can do various change and modification, therefore the protection model of the present invention without departing from the spirit and scope of the present invention
Enclosing be subject to what claims were defined.
Claims (7)
1. method that is a kind of while detecting 4 kinds of aflatoxin during liquor production in solid sample, which is characterized in that institute
The method of stating includes the following steps：
(1) it pre-processes：The solid sample to be measured after drying is weighed, sieving, the solid sample to be measured is vinasse, yeast or wine
Unstrained spirits；
(2) it extracts：Certain proportion water and acetonitrile is added, shakes mixing, obtains mixed liquor；
(3) it saltouts：Salting-out agents, concussion mixing centrifugation are added in mixed liquor；
(4) it purifies：Take the supernatant liquor in step (3) after centrifugation that cleanser, concussion centrifugation is added；
(5) it concentrates：0.22 μm of film is crossed after taking the supernatant liquor after centrifugation in step (4), nitrogen drying to redissolve；
(6) sample introduction is analyzed：Solution example after the middle film excessively of step (5) is subjected to UPLC-MS/MS detections.
2. according to the method described in claim 1, it is characterized in that, the method further includes being drawn with aflatoxin standard items
Thus standard curve calculates the content of aflatoxin in sample to be tested.
3. according to the method described in claim 1, it is characterized in that, in the step (2), the solid sample after being dried according to 5g
Add 10ml water and 15ml acetonitriles.
4. according to the method described in claim 1, it is characterized in that, the salting-out agents, are the solid-likes after being dried according to every 5g
Product add 1g NaCl and 4g MgSO4。
5. according to the method described in claim 1, it is characterized in that, chromatographic condition is in UPLC-MS/MS in the step (6)
Using C18 columns, mobile phase is A and B, and A is formic acid water, and B is methanol, using gradient elution.
6. according to the method described in claim 1, it is characterized in that, chromatographic condition is specifically in the UPLC-MS/MS：With
ACQUITY UPLC BEH C18 are chromatographic column；Using 0.01% formic acid water as mobile phase A phase, using 100% methanol as Mobile phase B
Phase, flow velocity 0.5ml/min；Type of elution is gradient elution, and elution program is as follows：0min, 5% Mobile phase B；7min, 60%
Mobile phase B；9min, 100% Mobile phase B；11.00min 100% Mobile phase B；11.10min 5% Mobile phase B；14.00min,
5% Mobile phase B.
7. according to the method described in claim 1, it is characterized in that, in the step (6) UPLC-MS/MS using electron spray from
Sub-ization source carries out data acquisition, ion source voltage 3kV using negative ions pattern, and ion source temperature is 150 DEG C, removes solvent
Temperature is 300 DEG C.
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| CN106526056B (en) * | 2017-01-04 | 2018-06-05 | 浙江国正检测技术有限公司 | AFB in beer and its supplementary material1Ultra performance liquid chromatography-tandem mass spectrum detection method |
| CN106950328B (en) * | 2017-03-27 | 2020-07-31 | 中山市食品药品检验所 | Method for detecting mycotoxin in fermented tea |
| CN107764614A (en) * | 2017-09-21 | 2018-03-06 | 四川省丹丹郫县豆瓣集团股份有限公司 | A kind of pre-treating method of bean paste aflatoxin B1 detection |
| CN108956801A (en) * | 2018-05-21 | 2018-12-07 | 安徽瑞思威尔科技有限公司 | The non-targeted quick screening method of unknown mycotoxin in a kind of white wine |
| CN117007712B (en) * | 2023-08-04 | 2024-03-26 | 安徽天祥药业有限公司 | Method for detecting aflatoxin in stir-fried stiff silkworm decoction pieces |
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