CN105784860A - Method for detecting aflatoxin of solid sample in baijiu production process - Google Patents
Method for detecting aflatoxin of solid sample in baijiu production process Download PDFInfo
- Publication number
- CN105784860A CN105784860A CN201610122255.4A CN201610122255A CN105784860A CN 105784860 A CN105784860 A CN 105784860A CN 201610122255 A CN201610122255 A CN 201610122255A CN 105784860 A CN105784860 A CN 105784860A
- Authority
- CN
- China
- Prior art keywords
- mobile phase
- aflatoxin
- uplc
- solid sample
- baijiu
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
-
- 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
- G01N30/06—Preparation
Abstract
The invention discloses a method for detecting aflatoxin of a solid sample in the baijiu production process, and belongs to the technical field of food detection.The method comprises the steps that after correlative pretreatment is carried out on baijiu distillers' grains, a UPLC-MS/MS detector is combined to detect existence of aflatoxin in the baijiu distillers' grains.A novel baijiu quality safety index detecting technology is provided, operation is easy and convenient, infinitesimal aflatoxin possibly existing in the baijiu distillers' grains can be fast monitored in time, and therefore the quality safety of baijiu is effectively controlled.
Description
Technical field
The present invention relates to the detection method of the aflatoxin of solid sample during a kind of liquor production, belong to food inspection
Survey technology field.
Background technology
Aflatoxin belongs to mycotoxin, is delimited as " first kind is carcinogenic by the Agency for Research on Cancer of World Health Organization (WHO)
Thing ".It easily pollutes cereal crops, meat and milk product etc., and hazardness is have destruction to make to people and animal livers tissue
With, time serious, may result in hepatocarcinoma the most dead.
Cereal crops are the main production raw material of Liquor-making industry, it is more likely that by aflatoxin and product poison microorganism band
Enter in Chinese liquor, threaten the safety of liquor production.The safety problem that food service industry occurs now is continuous, and about aflatoxin pair
Liquor production impact report almost without.Therefore, checking aflatoxin safety research in liquor production is very
Necessary.Going from strength to strength along with Spirits market simultaneously, it is also increasing for feed manufacturing industry, institute that its by-product loses grain
Also to seem particularly significant to losing the detection of aflatoxin in grain.
Detection object for aflatoxin is mainly Semen Maydis, Oryza glutinosa, Semen sojae atricolor, milk product, edible oil, flavoring agent at present
Deng；Fermentation drinks such as wine, medicated beer also has pertinent literature to report；Detection method focuses primarily upon thin layer chromatography, high-efficient liquid
Phase chromatography, euzymelinked immunosorbent assay (ELISA), Liquid Chromatography/Mass Spectrometry etc..Owing to liquor production process relates to plurality of raw materials, multiple-microorganism, and
The generation of multiple metabolite, so the solid sample during liquor production, such as Daqu (massive raw stater for alcholic liquor), fermented grain, distiller grains etc., with cereals etc.
Grain samples is compared, and is extremely complex, there is multiple not clear interfering material during detection.
But, the domestic research for Chinese liquor is the most less, has scholar to use ELISA method to detect Daqu (massive raw stater for alcholic liquor), and fermented grain loses grain, yellow
Water, base liquor, the AFB1 content in finished wine；Easily there is false positive in ELISA detection method, and testing result is bigger than normal, and not
The existence of multiple toxin can be detected simultaneously, accurately qualitative, quantitative checking is remained a need for for its experimental result.Also scholar is had to use
High performance liquid chromatography detection Sorghum vulgare Pers., Daqu (massive raw stater for alcholic liquor), fermented grain, yellow fluid, AFB1 content in finished wine, but this method is deposited
In detection time length, the problem such as susceptiveness is not enough, and can the kind of simultaneously detected aflatoxin few.
Therefore, develop a kind of quick, accurate, highly sensitive, with detecting sending out for Chinese liquor of multiple aflatoxin the most simultaneously
The detection method of the solid sample during ferment, is the problem needing solution at present badly.
Summary of the invention
In order to overcome the problems referred to above, during this method provides one based on detecting liquor production while UPLC-MS/MS
The detection method of 4 kinds of aflatoxin of solid sample, can realize the solid sample during liquor production quickly and easily,
The detection of aflatoxin in such as distiller grains.The method of the present invention is easy and simple to handle, the shortest, is applicable to batch samples simultaneously
Detection.The inventive method achieves and detects while aflatoxin AFB1, AFB2, AFG1, AFG2, and the response rate is high, steady
Qualitative preferably.
The detection method of the present invention, comprises the following steps:
(1) pretreatment: weigh the solid sample after drying, sieve；
(2) extract: add certain proportion water and solvent orange 2 A, concussion mixing, obtain mixed liquor；
(3) saltout: adding salting-out agents in mixed liquor, concussion mixing is centrifugal；
(4) purify: taking the supernatant after being centrifuged in step (3) and add cleanser, concussion is centrifugal；
(5) concentrating: take the supernatant after being centrifuged in step (4), nitrogen crosses 0.22 μm film after drying up redissolution；
(6) sample introduction analysis: the solution example after crossing film in step (5) carries out UPLC-MS/MS detection.
In one embodiment of the invention, during described solid sample is Chinese liquor distiller grains, or liquor production
Other solid samples, such as Daqu (massive raw stater for alcholic liquor), fermented grain.
Concrete, described step (1) is sieved into crossing 20 mesh sieves.
Preferably, in described step (2), solvent orange 2 A is acetonitrile.
Preferably, in described step (2), the solid sample after drying according to 5g adds 10ml water and 15ml acetonitrile.
Preferably, salting-out agents in described step (3), are that the solid sample after drying according to every 5g adds 1g NaCl and 4g
MgSO4。
Concrete, in described step (3), concussion mode is for manually to shake up and down, and the concussion time is 1min.
Preferably, cleanser in described step (4), be according to every 5g dry after solid sample add 150mg PSA and
900mg MgSO4。
Concrete, in described step (4), concussion mode is vortex oscillation, and the concussion time is 30s.
Concrete, centrifugation step in described step (3) and (4), parameter of noncentricity is 4000rpm rotating speed 5min.
Concrete, in described step (5), nitrogen dries up in redissolution step, redissolves liquid for flowing phase (mobile phase A and flowing
Phase B 1:1 by volume mixes), volume is 0.5mL.
Concrete, in described step (5), the solution example amount used by UPLC-MS/MS detection is 5 μ L.
Preferably, in described step (6), in UPLC-MS/MS, chromatographic condition is for using C18 post, and flowing is A and B mutually, and A is
Formic acid water, B is methanol, uses gradient elution.
Preferably, described mobile phase A and B, A flowing phase concentration is 0.01% (volume fraction), and flow velocity is 0.500ml/
min。
In one embodiment of the invention, described chromatographic condition is specifically: with ACQUITY UPLC BEH C18 be
Chromatographic column；With 0.01% formic acid water for mobile phase A phase, with 100% methanol for Mobile phase B phase, flow velocity is 0.5ml/min；Eluting
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, in described step (6), the Mass Spectrometry Conditions of UPLC-MS/MS is as follows: ion source is electro-spray ionization source
(ESI)；Spray voltage be 3000V (+)；Ion source temperature is 150 DEG C, and removing solvent temperature is 300 DEG C.
Wherein AFB1: parent ion is 313.10；Qualitative ion is 240.90, and collision energy is 35V；Quota ion is
268.70, collision energy is 32V；AFB2: parent ion is 315.10；Qualitative ion is 258.90, and collision energy is 35V；Quantitatively
Ion is 286.90, and collision energy is 25V；AFG1: parent ion is 329.10,；Qualitative ion is 242.80, and collision energy is
25V；Quota ion is 310.90, and collision energy is 20V；AFG2: parent ion is 331.10；Qualitative ion is 244.90, collision
Energy is 35V；Quota ion is 313.00, and collision energy is 24V.
In one embodiment of the invention, described method also includes drawing standard song with aflatoxin standard substance
Line, thus calculates the content of aflatoxin in distiller grains sample.
In one embodiment of the invention, described method specifically includes:
(1) extract: 5g distiller's dried grain powder (wet distiller grains dried 20 mesh sieves) adds the mixing of 10g water at low temperature, 15mL acetonitrile
Vortex shakes up 30s and extracts Aspergillus flavus poison poison；
(2) saltout: mixed liquor adds 1g NaCl and 4g MgSO4Concussion 1min, 4000rpm rotating speed 5min；Reduce mixed
Closing the saturated aqueous solution simultaneously of the water content in extracting solution promotes mixed liquor to be layered as acetonitrile layer and water layer；
(3) purify: step of learning from else's experience (2) saltout after supernatant, add scarvenger (150mg PSA, 900mg MgSO4) whirlpool
The even 30s of shaking by swirling, 4000rpm rotating speed 5min；
(4) concentrate: taking the supernatant after step (3) purifies, nitrogen redissolves after drying up to 1ml methanol: 0.1% formic acid water
(1:1), in solution, after 0.2 μm membrane filtration, 5 μ L sample introduction UPLC-MS/MS detection by quantitative are taken.
Beneficial effects of the present invention:
(1) the inventive method is to be applied to detection and the analysis of aflatoxin in Chinese liquor distiller grains first.The method is sensitive
Degree height, simple operation.Pre-treatment is simple to operation the shortest, by using Liquid Chromatography/Mass Spectrometry detection time (14min) ratio existing
High performance liquid chromatography detection the time (30min) shorter；The detection of AFB1 is limited to 0.09 μ g/kg, far below existing Chinese liquor sample
The detection limit that product examine is surveyed；Multiple aflatoxin can be detected simultaneously, including: AFB1, AFB2, AFG1, AFG2.
(2) can be applicable to the detection of aflatoxin in other solid samples in distiller grains and liquor production system.The present invention
Method carries out sample introduction analysis by UPLC-MS/MS to Chinese liquor distiller grains sample, detects the content of aflatoxin in Chinese liquor distiller grains,
Analysis speed is fast, decreases false positive simultaneously, improves the accuracy of mensuration, practical.The method is to yellow in Chinese liquor distiller grains
The detection of aspertoxin content has important directive significance, and the timely safety monitoring for liquor production system has guidance work
With.Advance food safety implementation of work in liquor production.
Accompanying drawing explanation
Fig. 1 is the separating effect figure of the lower 4 kinds of aflatoxin of chromatographic condition of the present invention.
Detailed description of the invention
Experiment material:
Triple level Four bar mass spectrograph (waters), the ACOUITY Ultra Performance LC chromatograph of liquid (U.S.
Waters company), ultrapure water machine (Millipore company of the U.S.), aflatoxin standard substance (Sigma company), acetonitrile, first
Alcohol, formic acid is chromatographically pure, PSA (Shanghai ANPEL Scientific Instrument Co., Ltd.).
Embodiment 1: the qualitative and quantitative detection of aflatoxin in distiller grains
Detect by the following method:
(1) extract: 5g distiller's dried grain powder (wet distiller grains dried 20 mesh sieves) adds the mixing of 10g water at low temperature, 15mL acetonitrile
Vortex shakes up 30s and extracts Aspergillus flavus poison poison；
(2) saltout: mixed liquor adds 1g NaCl and 4g MgSO4Concussion 1min, 4000rpm rotating speed 5min；Reduce mixed
Closing the saturated aqueous solution simultaneously of the water content in extracting solution promotes mixed liquor to be layered as acetonitrile layer and water layer；
(3) purify: step of learning from else's experience (2) saltout after supernatant, add scarvenger (150mg PSA, 900mg MgSO4) whirlpool
The even 30s of shaking by swirling, 4000rpm rotating speed 5min；
(4) concentrate: taking the supernatant after step (3) purifies, nitrogen redissolves after drying up to 1ml methanol: 0.1% formic acid water
(1:1), in solution, after 0.2 μm membrane filtration, 5 μ L sample introduction UPLC-MS/MS detection by quantitative are gone.
The wherein chromatographic condition of UPLC-MS/MS: ACQUITY UPLC BEH C18；With 0.01% formic acid as mobile phase A
Phase, with 100% methanol for Mobile phase B phase, flow velocity is 0.5mL/min；Eluting, eluting journey is carried out by the gradient elution mode of table 1
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 this chromatographic condition, 4 kinds of aflatoxin can
It is kept completely separate and peak shape is preferable (as shown in Figure 1).
Table 1 eluent gradient
Wherein the Mass Spectrometry Conditions of UPLC-MS/MS is: ion source is electro-spray ionization source (ESI)；Spray voltage is
3000V(+)；Ion source temperature is 150 DEG C, and removing solvent temperature is 300 DEG C.
Wherein AFB1: parent ion is 313.10；Qualitative ion is 240.90, and collision energy is 35V；Quota ion is
268.70, collision energy is 32V；AFB2: parent ion is 315.10；Qualitative ion is 258.90, and collision energy is 35V；Quantitatively
Ion is 286.90, and collision energy is 25V；AFG1: parent ion is 329.10,；Qualitative ion is 242.80, and collision energy is
25V；Quota ion is 310.90, and collision energy is 20V；AFG2: parent ion is 331.10；Qualitative ion is 244.90, collision
Energy is 35V；Quota ion is 313.00, and collision energy is 24V.
Through above step, contrasted by the appearance time with aflatoxin standard substance, i.e. achieve the Huang in sample
The qualitative detection of aspertoxin.It addition, by using the aflatoxin standard substance of known quantity to draw standard curve, by target peak
Area substitutes in standard curve, can obtain the content of corresponding aflatoxin in sample introduction sample, and then know that Chinese liquor is raw
The content of the aflatoxin in solid sample during product, i.e. realizes aflatoxin AFB1, AFB2, AFG1, AFG2
Detection by quantitative.In addition to distiller grains sample, the inventive method can also be used to detect Daqu (massive raw stater for alcholic liquor), fermented grain sample.
Embodiment 2: the quantitative detecting method study on the efficiency of the present invention
Accurately weigh 5g distiller's dried grain end, be separately added into different volumes standard substance mixed solution, enter according to the method for embodiment 1
Row detection, makes respective standard curve, and concrete concentration is shown in Table 2 to table 5.
Table 2 AFB1 standard curve concentration
Table 3 AFB2 standard curve concentration
Table 4 AFG1 standard curve concentration
Table 5AFG2 standard curve concentration
The above-mentioned each 5ul of serial solution standard solution of accurate absorption, sample introduction analysis, record each component chromatographic peak area to be measured,
With sample introduction concentration as abscissa (X), peak area is vertical coordinate (Y), carries out regression analysis, and result (being shown in Table 6) shows, each component lines
Sexual relationship is good.
Table 6 AFB1, B2, G1, G2 regression equation and correlation coefficient
Meanwhile, the detection limit of the inventive method, quantitative limit, the response rate, stability data are as shown in table 7 to table 10.Except
Outside distiller grains sample, using the inventive method to detect Daqu (massive raw stater for alcholic liquor), fermented grain sample, standard curve linear dependence is also fine, inspection
Rising limit, quantitative limit, the response rate and stability are also similar with distiller grains sample.
Table 7 AFB1, B2, G1, G2 detection limit parameter value
Table 8 AFB1, B2, G1, G2 quantitative limit parameter value
Table 9 AFB1, B2, G1, G2 response rate experiment parameter value
Table 10 AFB1, B2, G1, G2 stability (RSD) parameter value
Embodiment 3: the testing conditions impact on testing result
The present invention also compares the impact on Detection results of the different disposal method.
(1) impact of sample state: replacing dry crushing distiller grains as sample with wet distiller grains, other steps are consistent with embodiment 1.
Result shows, the content of the aflatoxin eventually detected reduces about 35% than embodiment 1, the stability of detection and recovery
Rate receives and has a strong impact on, and cannot realize the effective detection to aflatoxin at all.
(2) impact of Extraction solvent: replacing acetonitrile as Extraction solvent with methanol, other steps are consistent with embodiment 1.Knot
Fruit display, the content of the aflatoxin eventually detected reduces about 22% than embodiment 1, the stability of detection and the response rate
Receive and have a strong impact on.Additionally, inventor also finds, directly use acetonitrile when Extraction solvent does not add water, the Huang eventually detected
The content of aspertoxin reduces about 60% than the combination using acetonitrile and water, illustrates to use acetonitrile and water combination molten as extracting
Agent can significantly improve the accuracy of detection.
(3) impact purified: omit the purified treatment in embodiment 1 step (3), found that eventually detect is yellow bent
The content of mould toxin reduces about 43% than embodiment 1, and the stability of detection and the response rate receive and have a strong impact on.This also illustrates this
The purifying treatment method of invention can significantly improve the accuracy of detection.
(4) impact of liquid phase process: use 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 can not be kept completely separate by the peak shape presented in collection of illustrative plates.
Although the present invention is open the most as above with preferred embodiment, but it is not limited to the present invention, any is familiar with this skill
The people of art, without departing from the spirit and scope of the present invention, can do various changes and modification, therefore the protection model of the present invention
Enclosing should be with being as the criterion that claims are defined.
Claims (9)
1. the method for 4 kinds of aflatoxin in solid sample during detection liquor production simultaneously, it is characterised in that institute
The method of stating comprises the following steps:
(1) pretreatment: weigh the solid sample to be measured after drying, sieve；
(2) extract: add certain proportion water and solvent orange 2 A, concussion mixing, obtain mixed liquor；
(3) saltout: adding salting-out agents in mixed liquor, concussion mixing is centrifugal；
(4) purify: taking the supernatant after being centrifuged in step (3) and add cleanser, concussion is centrifugal；
(5) concentrating: take the supernatant after being centrifuged in step (4), nitrogen crosses 0.22 μm film after drying up redissolution；
(6) sample introduction analysis: the solution example after crossing film in step (5) carries out UPLC-MS/MS detection.
Method the most according to claim 1, it is characterised in that described method also includes drawing with aflatoxin standard substance
Standard curve, thus calculates the content of aflatoxin in testing sample.
Method the most according to claim 1, it is characterised in that the solvent orange 2 A of described step (2) is acetonitrile.
Method the most according to claim 1, it is characterised in that in described step (2), the solid sample after drying according to 5g
Add 10ml water and 15ml acetonitrile.
Method the most according to claim 1, it is characterised in that described salting-out agents, is the solid-like after drying according to every 5g
Product add 1g NaCl and 4g MgSO4。
Method the most according to claim 1, it is characterised in that in described step (6), in UPLC-MS/MS, chromatographic condition is
Use C18 post, flowing be mutually A and B, A be formic acid water, B is methanol, employing gradient elution.
Method the most according to claim 1, it is characterised in that in described UPLC-MS/MS, chromatographic condition is specifically: with
ACQUITY UPLC BEH C18 is chromatographic column；With 0.01% formic acid water for mobile phase A phase, with 100% methanol as Mobile phase B
Phase, flow velocity is 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.
Method the most according to claim 1, it is characterised in that in described step (6) UPLC-MS/MS use electron spray from
Sub-ization source, uses negative ions pattern to carry out data acquisition, and ion source voltage is 3kV, and ion source temperature is 150 DEG C, removes solvent
Temperature is 300 DEG C.
Method the most according to claim 1, it is characterised in that described solid sample to be measured is distiller grains, Daqu (massive raw stater for alcholic liquor) or fermented grain.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610122255.4A CN105784860B (en) | 2016-03-03 | 2016-03-03 | The detection method of the aflatoxin of solid sample during a kind of liquor production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610122255.4A CN105784860B (en) | 2016-03-03 | 2016-03-03 | The detection method of the aflatoxin of solid sample during a kind of liquor production |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105784860A true CN105784860A (en) | 2016-07-20 |
| CN105784860B CN105784860B (en) | 2018-08-07 |
Family
ID=56387954
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610122255.4A Active CN105784860B (en) | 2016-03-03 | 2016-03-03 | The detection method of the aflatoxin of solid sample during a kind of liquor production |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105784860B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106526056A (en) * | 2017-01-04 | 2017-03-22 | 浙江国正检测技术有限公司 | Ultra-high performance liquid chromatography and tandem mass spectrometry detection method for AFB1 in beer and raw and auxiliary materials of beer |
| CN106950328A (en) * | 2017-03-27 | 2017-07-14 | 中山市食品药品检验所 | A kind of 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 |
| CN117007712A (en) * | 2023-08-04 | 2023-11-07 | 安徽天祥药业有限公司 | Method for detecting aflatoxin in stir-fried stiff silkworm decoction pieces |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1588068A (en) * | 2004-09-07 | 2005-03-02 | 上海大学 | Detecting method for aflatoxins |
| CN101655480A (en) * | 2009-07-24 | 2010-02-24 | 合肥工业大学 | Method for rapidly detecting aflatoxin content |
| CN102338789A (en) * | 2011-04-22 | 2012-02-01 | 上海谱尼测试技术有限公司 | Fast instrumental analysis method for aflatoxins in foods |
-
2016
- 2016-03-03 CN CN201610122255.4A patent/CN105784860B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1588068A (en) * | 2004-09-07 | 2005-03-02 | 上海大学 | Detecting method for aflatoxins |
| CN101655480A (en) * | 2009-07-24 | 2010-02-24 | 合肥工业大学 | Method for rapidly detecting aflatoxin content |
| CN102338789A (en) * | 2011-04-22 | 2012-02-01 | 上海谱尼测试技术有限公司 | Fast instrumental analysis method for aflatoxins in foods |
Non-Patent Citations (6)
| Title |
|---|
| LUKAS VACLAVIK ET AL.: "Analysis of multiple mycotoxins in cereals under ambient conditions using direct analysis in real time (DART) ionization coupled to high resolution mass spectrometry", 《TALANTA》 * |
| M. ZACHARIASOVA ET AL.: "Novel approaches in analysis of Fusarium mycotoxins in cereals employing ultra performance liquid chromatography coupled with high resolution mass spectrometry", 《ANALYTICA CHIMICA ACTA》 * |
| VOJISLAVA P. BURSIC ET AL.: "ANALYSIS OF AFLATOXINS B1 AND G1 IN MAIZE BY QUECHERS", 《JOUR. NAT. SCI》 * |
| YONGGANG LI ET AL.: "Ultra-high performance liquid chromatography tandem mass spectrometry for simultaneous analysis of aflatoxins B1, G1, B2, G2, zearalenone and its metabolites in eggs using a QuEChERS-based extraction procedure", 《ANAL. METHODS》 * |
| 杨振宇 等: "进口玉米酒糟粕中15种真菌毒素的检测和风险分析", 《中国粮油学报》 * |
| 胡文彦 等: "基于QuEChEＲS提取的快速液相色谱-串联质谱法测定婴幼儿谷基辅助食品中的9种真菌毒素", 《色谱》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106526056A (en) * | 2017-01-04 | 2017-03-22 | 浙江国正检测技术有限公司 | Ultra-high performance liquid chromatography and tandem mass spectrometry detection method for AFB1 in beer and raw and auxiliary materials of beer |
| CN106950328A (en) * | 2017-03-27 | 2017-07-14 | 中山市食品药品检验所 | A kind of 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 |
| CN117007712A (en) * | 2023-08-04 | 2023-11-07 | 安徽天祥药业有限公司 | Method for detecting aflatoxin in stir-fried stiff silkworm decoction pieces |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105784860B (en) | 2018-08-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105784860A (en) | Method for detecting aflatoxin of solid sample in baijiu production process | |
| CN104535664B (en) | A kind of method simultaneously detecting multiple mycotoxin in sesame paste | |
| CN105954454A (en) | Method for separating and assaying organic acid and fatty acid substances in saliva | |
| CN105536746B (en) | A kind of SPME capsule and its detection beverage in phenols environmental estrogens application | |
| CN107727781A (en) | Solid-phase extraction column that is a kind of while purifying a variety of mycotoxins and its application | |
| CN105445390B (en) | The detection method that chloromycetin remains in dairy products | |
| CN105148558A (en) | Solid-phase extraction column for purifying fungaltoxin and application of solid-phase extraction column | |
| CN106546679A (en) | The liquid phase chromatography analytical method of acrylamide in a kind of detection fried food | |
| CN105954422A (en) | Method for quick detection of content of citrinin in traditional Chinese medicinal materials | |
| CN106645477B (en) | A kind of remaining method of detection florfenicol amine and application | |
| CN106596785A (en) | Method for rapidly measuring fusarium toxins in cereal grains | |
| CN109030665A (en) | The detection method of beet alkali content in hydrophilic liquid phase chromatographic tandem mass spectrometric determination red beet | |
| CN108445128A (en) | A kind of method of carbamates determination of drug residues in birds, beasts and eggs | |
| CN106526056B (en) | AFB in beer and its supplementary material1Ultra performance liquid chromatography-tandem mass spectrum detection method | |
| CN106770783B (en) | A kind of method that liquid-liquid micro-extraction closes 9 kinds of aromatic amines in phase chromatographic tandem mass spectrography detection cigarette mainstream flue gas | |
| CN103257195B (en) | GC-MS/MS (Gas chromatography-tandem mass spectrometry) method for simultaneously analyzing benzo [a] BaA, chrysene and benzo [a] BaP in main stream smoke of cigarettes | |
| CN103217498A (en) | Method for detecting dicyandiamide in milk powder with LC-MS (liquid chromatography/mass spectrometry) and sample preparation method | |
| CN204789501U (en) | A multi -functional decontaminating column that is used for chain check spore toxin to detect | |
| CN109541088A (en) | A kind of purification method of patulin, solid-phase extraction column and its application | |
| CN105954434A (en) | Method for detecting phenols spice | |
| CN107037155B (en) | Simultaneously in extracting and enriching gauge water typical four kinds of Taste and odor compounds and three kinds of algae toxins method | |
| CN104977383A (en) | Method for rapidly and quantitatively detecting microcystins in spirulina food | |
| Du et al. | Determination of 43 pesticide residues in intact grape berries (Vitis vinifera L.) by using an ultrasound-assisted acetonitrile extraction method followed by LC–MS/MS | |
| CN107589204A (en) | The method of Anthranilate class grape essence in GC-MS measure grape wine | |
| CN106706824B (en) | The detection method of juvenile hormone JH II in a kind of insect bodies of application of gas chromatorgraphy/mass |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |