CN107271591A - A kind of method extracted and detect citrinin toxin in preserved red beancurd - Google Patents
A kind of method extracted and detect citrinin toxin in preserved red beancurd Download PDFInfo
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Abstract
The invention belongs to detection field, there is provided a kind of method extracted and detect citrinin toxin in preserved red beancurd, including step：1) preserved red beancurd sample and methanol are mixed, reaction extracts citrinin toxin soiutions；Wherein the mass volume ratio of preserved red beancurd sample and methanol is 1g：5mL；2) obtained citrinin toxin soiutions high performance liquid chromatography detection is extracted.The present invention is soluble in acetonitrile, methanol, ethyl acetate, the physicochemical property of acetone and other organic solvent using citrinin, proposes a kind of more easy method for extracting citrinin toxin in preserved red beancurd, is conducive to the development of promotion red yeast rice and red yeast rice industry.The method of the present invention being capable of citrinin toxin in rapid extraction preserved red beancurd, and efficiency high, it is time-consuming less, cost is low, the rate of recovery is high, meet Good Laboratory control specification food Physico-chemical tests standard, in addition, the extraction of citrinin toxin, is worth with high promotion and application in the also greatly easy red yeast rice of the method and its Related product.
Description
Technical field
The invention belongs to detection field, and in particular to a kind of extraction and the method for detecting citrinin toxin.
Background technology
Citrinin is mainly as a kind of secondary metabolite produced by Penicillium, aspergillus, monascus.Citrinin point
Cloth extensively, is primarily present in the bread baskets such as wheat, corn, oat, and the fabricated product of apple, pear and other fruits.Tangerine is mould
Element has good biocidal property, can suppress bacillus subtilis, staphylococcus aureus, Escherichia coli, streptomyces griseus etc.,
Ancient Times in China is just applied on perishable meat as a kind of food preservation agent.But have very strong renal toxicity due to citrinin and
Not by extensive use, and its pollution problem is increasingly paid close attention to by people, and naturally malicious by international school of life and health sciences
European branch of the plain detection committee is classified as one of the toxin that must detect.
China is red yeast rice production in the world with using earliest, most wide country, just making red using monascus early in the Ming Dynasty
It is bent.And preserved red beancurd is main using rice as raw material, by Fermentation Condition of Monascus spp.Because preserved red beancurd not only can be with promoting blood circulation and removing blood stasis, invigorating the spleen
Help digestion, can more reduce blood glucose cholesterol, early in《Compendium of Materia Medica》In just have a large amount of records, and all the time by it is both domestic and external extensively
Concern.Citrinin content of toxins also turns into the main contents of China's monascus product export inspection quarantine in preserved red beancurd.Domestic and international base
Contained citrinin content of toxins set up different limitation standards in different detection methods is to agricultural product, food, feed,
With the constantly improve of HPLC technologies, detection work is increasingly simple, and the pre-treatment of sample is into key problem in technology and difficult point.At present
It is complex for citrinin toxin isolation and purification method, all it is generally to realize citrinin toxin point by concentrating, crossing post, extraction
From finally by TLC or HPLC progress qualitative and quantitative detections.
The content of the invention
The problem of existing for this area, extracts and detects citrinin poison in preserved red beancurd the purpose of the present invention is to propose to one kind
The method of element.
The technical scheme for realizing the object of the invention is：
A kind of method extracted and detect citrinin toxin in preserved red beancurd, including step：
1) preserved red beancurd sample and methanol are mixed, reaction extracts citrinin toxin soiutions；Wherein preserved red beancurd sample and first
The mass volume ratio of alcohol is 1g：(5-20mL)；
2) step 1) extract obtained citrinin toxin soiutions high performance liquid chromatography (HPLC) detection.
Wherein, the methanol is hplc grade methanol.I.e. undiluted hplc grade methanol.
Preferably, the methanol is hplc grade methanol, and the mass volume ratio of preserved red beancurd sample and methanol is 1g：5mL.
Wherein, step 1) in, after preserved red beancurd sample and methanol are mixed, at room temperature with 100~300rpm speed oscillations 30~
120min, then centrifuge, it is citrinin toxin soiutions to take supernatant.
Wherein, the rotating speed of the centrifugation is 7000~10000rpm, and the time of centrifugation is 8~15min.
Wherein, step 2) in, the condition of high performance liquid chromatography is：Chromatographic column：Agilent TC-C18,4.6 × 250mm, 5
μm；Acetonitrile/isopropanol/0.08mol/L phosphoric acid solutions that mobile phase is, the volume ratio of acetonitrile/isopropanol/0.08mol/L phosphoric acid
For 35：10：55.
Wherein, step 2) in, detected with fluorescence detector, Detection wavelength is that 331nm excitation wavelengths and 500nm launch
Wavelength；Flow velocity is 1.0mL/min；40 DEG C of column temperature；The μ L of sample size 50.
Wherein, step 2) eluent at the peak consistent with citrinin toxin standard items retention time is collected, using external standard method
Quantitative determined, obtain the citrinin content of toxins in preserved red beancurd sample, the retention time is front and rear 0.05min.
Specifically, hplc grade methanol is dissolved in citrinin standard items, is configured to the standard of 0.01~10 μ g/g series concentrations
Curve working solution.HPLC is carried out using high performance liquid chromatography to the standard curve working solution of various concentrations quantitatively to detect, and with
Citrinin concentration makees abscissa, and ordinate is made with the peak area at 0.05min before and after retention time, according to concentration and peak area
Relation carries out linear regression, standard curve is drawn, for external standard method.
The beneficial effects of the present invention are：
Method proposed by the present invention, acetonitrile, methanol, ethyl acetate, acetone and other organic solvent are soluble in using citrinin
Physicochemical property, has invented a kind of more easy method for extracting citrinin toxin in preserved red beancurd, be conducive to promoting red yeast rice and
The development of red yeast rice industry.Tests prove that, method of the invention can citrinin toxin in rapid extraction and detection preserved red beancurd, and
Efficiency high, it is time-consuming less, cost is low, high (0.1-1 μ g/g, rate of recovery scope is in 80-110% for the rate of recovery；1-100 μ g/g, the rate of recovery
Scope is in 90-110%), meet Good Laboratory control specification-food Physico-chemical tests standard (GB/T 27404), in addition, this side
The extraction of citrinin toxin, is worth with high promotion and application in the also greatly easy red yeast rice of method and its Related product.
Brief description of the drawings
Fig. 1 is citrinin content of toxins examination criteria curve spectrum.
Fig. 2 is the HPLC collection of illustrative plates of 2 μ g/g citrinin toxin standard items.
Fig. 3 is to extract the HPLC collection of illustrative plates that citrinin content of toxins is 0.54 μ g/g in preserved red beancurd sample A using this method；
Fig. 4 is to extract the HPLC figures that citrinin content of toxins is 0.57 μ g/g in preserved red beancurd sample A using immune affinity column
Spectrum.
Embodiment
Now illustrate the present invention with following examples, but be not limited to the scope of the present invention.The hand used in embodiment
Section, unless otherwise instructed, using the conventional means in this area.
Experimental method used in following embodiments is conventional method unless otherwise specified.
Material, reagent used etc., unless otherwise specified, are commercially obtained in following embodiments.
Quantitative test in following embodiments, is respectively provided with three repetition experiments, results averaged.
Citrinin standard items in following embodiments are the products in Sigma companies (U.S.).The methanol of chromatographic grade, acetonitrile,
Isopropanol and phosphoric acid are the products in Fisher companies (U.S.).
The preparation method of citrinin standard curve is as follows：
With the molten 1mg solids citrinin standard items of 1mL hplc grade methanols, 1mg/g citrinin standard liquids are configured to, then use color
Spectrum level methanol is configured to 2 μ g/g, 1 μ g/g, 0.5 μ g/g, 0.1 μ g/g, 0.05 μ g/g, the work of 0.01 μ g/g standard curves respectively
Liquid.HPLC is carried out using high performance liquid chromatography to the standard curve working solution of various concentrations quantitatively to detect, and it is dense with citrinin
Degree makees abscissa, and ordinate is made with the peak area at 0.05min before and after retention time, is carried out according to concentration and the relation of peak area
Linear regression, and draw standard curve.
High performance liquid chromatography condition：Chromatographic column：Agilent TC-C18,4.6 × 250mm, 5 μm；Mobile phase：Acetonitrile/
Isopropanol/0.08mol/L phosphoric acid (35/10/55, V/V/V)；Fluorescence detector：Agilent G1321；Detection wavelength：331nm and
500nm；Flow velocity：1.0mL/min；40 DEG C of column temperature；Sample size：50μL.
The standard curve of drafting is as shown in Figure 1.It is according to the calibration curve equation that standard curve is obtained：Y=
206.631416x+0.6943595 (y is peak area, and x is citrinin content of toxins), R2=0.99924.Fig. 2 is that 2 μ g/g tangerines are mould
The HPLC collection of illustrative plates of plain toxin standard items.
It is as follows that citrinin content of toxins step in preserved red beancurd sample is extracted using immune affinity column：
Take 1g crush after sample, add the methanol of 20mL 70%, 65 DEG C of water-bath 30min (turn upside down 30s per 10min),
Filtered with qualitative filter paper；Take 1mL filtrates to 50mL centrifuge tubes, add 39mL PBSs, filtered with microfibre filter paper；Take
The above-mentioned filtrates of 10mL cross post, and wash post with the Tween-20-PBS of 10mL 0.1%, finally with 1mL eluent (methanol：0.1% phosphoric acid
=7：3) cross post citrinin is eluted in dose jar；Carry out HPLC quantitatively to detect, data processing is carried out with quantified by external standard method.It is red
Fermented bean curd sample is repeated 3 times, and is averaged.
Embodiment 1：Extract the method for citrinin toxin and the detection of citrinin content of toxins in preserved red beancurd
It is utilized respectively 2 kinds of methods and citrinin Toxic extraction is carried out to preserved red beancurd sample A, then carries out HPLC and quantitatively detect.
Comprise the following steps that：
1st, citrinin content of toxins in preserved red beancurd is extracted using the inventive method
It is accurate to weigh the preserved red beancurd sample A that 1g has fully mixed (stirring and evenly mixing), it is placed in 50mL centrifuge tubes, adds 5mL
Hplc grade methanol, room temperature is placed on shaking table, and 200rpm is acutely shaken after 60min, and 8000rpm centrifugation 10min, standing takes supernatant
Into 2mL micro-samplings bottle, efficient liquid phase chromatographic analysis (Fig. 3) is carried out to sample liquid using high performance liquid chromatography (HPLC),
Data processing is carried out with quantified by external standard method.Preserved red beancurd sample A is repeated 3 times, and is averaged.
2nd, citrinin content of toxins in preserved red beancurd is extracted by the use of immune affinity column as control
The preserved red beancurd sample A that 1g has fully been mixed accurately is weighed, is placed in 50mL centrifuge tubes, the methanol of 20mL 70% is added,
65 DEG C of water-bath 30min (turn upside down 30s per 10min), are filtered with qualitative filter paper.Take 1mL filtrates to 50mL centrifuge tubes, add
39mL PBSs, are filtered with microfibre filter paper.The above-mentioned filtrates of 10mL are taken to cross post, and with the Tween-20-PBS of 10mL 0.1%
Post is washed, finally with 1mL eluent (methanol：0.1% phosphoric acid=7：3) cross post citrinin is eluted in dose jar.Using efficient
Liquid chromatography (HPLC) carries out efficient liquid phase chromatographic analysis to sample liquid, and data processing is carried out with quantified by external standard method.Preserved red beancurd
Sample A is repeated 3 times, and is averaged.Fig. 4 is to extract citrinin content of toxins in preserved red beancurd sample A using immune affinity column to be
563.82 μ g/g HPLC collection of illustrative plates.
High performance liquid chromatography condition：Chromatographic column：Agilent TC-C18,4.6 × 250mm, 5 μm；Mobile phase：Acetonitrile/
Isopropanol/phosphoric acid (0.08mol/L) (35/10/55, V/V/V)；Fluorescence detector：Agilent G1321；Detection wavelength：331nm
And 500nm；Flow velocity：1.0mL/min；40 DEG C of column temperature；Sample size：50μL.
The eluent at the peak consistent with citrinin toxin standard items retention time (retention time about 0.05min) is collected, is obtained
To the citrinin content of toxins in preserved red beancurd sample A.
Testing result is as shown in table 1.Wherein, processing sample 1-3 is mould using tangerine in this method extraction 1g preserved red beancurd samples
Plain content of toxins；Processing control 1-3 is to extract citrinin content of toxins in 1g preserved red beancurd samples using immune affinity column；Citrinin
Content of toxins (μ g/g) is the actually detected value of citrinin content of toxins in 1g preserved red beancurd samples；Average value (μ g/g) is the red corruption of 1g
3 repetitions detect the average value of citrinin content of toxins in milk sample product；The rate of recovery (%) is sample detection average value (μ g/g)/right
According to detection average value (μ g/g) * 100%.
It is 0.55 μ g/g to extract citrinin content of toxins average value in 1g preserved red beancurd samples using this method；Utilize immune parent
It is 0.56 μ g/g to extract citrinin content of toxins average value in 1g preserved red beancurd samples with post, and the rate of recovery is 98.21% (0.55 μ g/
g/0.56μg/g).The above rate of recovery meets Good Laboratory control specification-food Physico-chemical tests standard (GB/T 27404)
(0.1-1 μ g/g, rate of recovery scope is in 80-110%；1-100 μ g/g, rate of recovery scope is in 90-110%), illustrate that the present invention is carried
The method of the citrinin toxin taken is correct, and this method is easier.
Citrinin content of toxins is detected in the preserved red beancurd sample A of table 1
Embodiment 2 extracts the method for citrinin toxin and the detection of citrinin content of toxins in preserved red beancurd
It is utilized respectively 2 kinds of methods and citrinin Toxic extraction is carried out to preserved red beancurd sample B, then carries out HPLC and quantitatively detect.
Comprise the following steps that：
1st, citrinin content of toxins in preserved red beancurd is extracted using this method
The preserved red beancurd sample B that 1g has fully been mixed accurately is weighed, is placed in 50mL centrifuge tubes, 5mL hplc grade methanols are added,
Room temperature place shaking table on, 200rpm is acutely shaken after 60min, 8000rpm centrifugation 10min, standing take supernatant to 2mL it is micro enter
In sample bottle, efficient liquid phase chromatographic analysis is carried out to sample liquid using high performance liquid chromatography (HPLC), carried out with quantified by external standard method
Data processing.Preserved red beancurd sample B is repeated 3 times, and is averaged.
2nd, citrinin content of toxins in preserved red beancurd is extracted by the use of immune affinity column as control
The preserved red beancurd sample B that 1g has fully been mixed accurately is weighed, is placed in 50mL centrifuge tubes, the methanol of 20mL 70% is added,
65 DEG C of water-bath 30min (turn upside down 30s per 10min), are filtered with qualitative filter paper.Take 1mL filtrates to 50mL centrifuge tubes, add
39mL PBSs, are filtered with microfibre filter paper.The above-mentioned filtrates of 10mL are taken to cross post, and with the Tween-20-PBS of 10mL 0.1%
Post is washed, finally with 1mL eluent (methanol：0.1% phosphoric acid=7：3) cross post citrinin is eluted in dose jar.Using efficient
Liquid chromatography (HPLC) carries out efficient liquid phase chromatographic analysis to sample liquid, and data processing is carried out with quantified by external standard method.Preserved red beancurd
Sample B is repeated 3 times, and is averaged.
High performance liquid chromatography condition：Chromatographic column：Agilent TC-C18,4.6 × 250mm, 5 μm；Mobile phase：Acetonitrile/
Isopropanol/phosphoric acid (0.08mol/L) (35/10/55, V/V/V)；Fluorescence detector：Agilent G1321；Detection wavelength：331nm
And 500nm；Flow velocity：1.0mL/min；40 DEG C of column temperature；Sample size：50μL.
The eluent at the peak consistent with citrinin toxin standard items retention time (retention time about 0.05min) is collected, is obtained
To the citrinin content of toxins in preserved red beancurd sample D.
Testing result is as shown in table 2.Wherein, processing sample 1-3 is mould using tangerine in this method extraction 1g preserved red beancurd samples
Plain content of toxins；Processing control 1-3 is to extract citrinin content of toxins in 1g preserved red beancurd samples using immune affinity column；Citrinin
Content of toxins (μ g/g) is the actually detected value of citrinin content of toxins in 1g preserved red beancurd samples；Average value (μ g/g) is the red corruption of 1g
3 repetitions detect the average value of citrinin content of toxins in milk sample product；The rate of recovery (%) is sample detection average value (μ g/g)/right
According to detection average value (μ g/g) * 100%.
It is 1.11 μ g/g to extract citrinin content of toxins average value in 1g preserved red beancurd samples using this method；Utilize immune parent
It is 1.16 μ g/g to extract citrinin content of toxins average value in 1g preserved red beancurd samples with post, and the rate of recovery is 95.69% (1.11 μ g/
g/1.16μg/g).The above rate of recovery meets Good Laboratory control specification-food Physico-chemical tests standard (GB/T 27404)
(0.1-1 μ g/g, rate of recovery scope is in 80-110%；1-100 μ g/g, rate of recovery scope is in 90-110%), illustrate that the present invention is carried
The method of the citrinin toxin taken is correct, and this method is easier.
Citrinin content of toxins is detected in the preserved red beancurd sample B of table 2
The method of citrinin toxin and the detection of citrinin content of toxins in embodiment 3, extraction preserved red beancurd
It is utilized respectively 2 kinds of methods and citrinin Toxic extraction is carried out to preserved red beancurd sample C, then carries out HPLC and quantitatively detect.
Comprise the following steps that：
1st, citrinin content of toxins in preserved red beancurd is extracted using this method
The preserved red beancurd sample C that 1g has fully been mixed accurately is weighed, is placed in 50mL centrifuge tubes, 5mL hplc grade methanols are added,
Room temperature place shaking table on, 200rpm is acutely shaken after 60min, 8000rpm centrifugation 10min, standing take supernatant to 2mL it is micro enter
In sample bottle, efficient liquid phase chromatographic analysis is carried out to sample liquid using high performance liquid chromatography (HPLC), carried out with quantified by external standard method
Data processing.Preserved red beancurd sample C is repeated 3 times, and is averaged.
2nd, citrinin content of toxins in preserved red beancurd is extracted by the use of immune affinity column as control
The preserved red beancurd sample C that 1g has fully been mixed accurately is weighed, is placed in 50mL centrifuge tubes, the methanol of 20mL 70% is added,
65 DEG C of water-bath 30min (turn upside down 30s per 10min), are filtered with qualitative filter paper.Take 1mL filtrates to 50mL centrifuge tubes, add
39mL PBSs, are filtered with microfibre filter paper.The above-mentioned filtrates of 10mL are taken to cross post, and with the Tween-20-PBS of 10mL 0.1%
Post is washed, finally with 1mL eluent (methanol：0.1% phosphoric acid=7：3) cross post citrinin is eluted in dose jar.Using efficient
Liquid chromatography (HPLC) carries out efficient liquid phase chromatographic analysis to sample liquid, and data processing is carried out with quantified by external standard method.Preserved red beancurd
Sample C is repeated 3 times, and is averaged.
High performance liquid chromatography condition：Chromatographic column：Agilent TC-C18,4.6 × 250mm, 5 μm；Mobile phase：Acetonitrile/
Isopropanol/phosphoric acid (0.08mol/L) (35/10/55, V/V/V)；Fluorescence detector：Agilent G1321；Detection wavelength：331nm
And 500nm；Flow velocity：1.0mL/min；40 DEG C of column temperature；Sample size：50μL.
The eluent at the peak consistent with citrinin toxin standard items retention time (retention time about 0.05min) is collected, is obtained
To the citrinin content of toxins in preserved red beancurd sample D.
Testing result is as shown in table 3.Wherein, processing sample 1-3 is mould using tangerine in this method extraction 1g preserved red beancurd samples
Plain content of toxins；Processing control 1-3 is to extract citrinin content of toxins in 1g preserved red beancurd samples using immune affinity column；Citrinin
Content of toxins (μ g/g) is the actually detected value of citrinin content of toxins in 1g preserved red beancurd samples；Average value (μ g/g) is the red corruption of 1g
3 repetitions detect the average value of citrinin content of toxins in milk sample product；The rate of recovery (%) is sample detection average value (μ g/g)/right
According to detection average value (μ g/g) * 100%.
It is 9.16 μ g/g to extract citrinin content of toxins average value in 1g preserved red beancurd samples using this method；Utilize immune parent
It is 9.44 μ g/g to extract citrinin content of toxins average value in 1g preserved red beancurd samples with post, and the rate of recovery is 98.09% (9.16 μ g/
g/9.44μg/g).The above rate of recovery meets Good Laboratory control specification-food Physico-chemical tests standard (GB/T 27404)
(0.1-1 μ g/g, rate of recovery scope is in 80-110%；1-100 μ g/g, rate of recovery scope is in 90-110%), illustrate that the present invention is carried
The method of the citrinin toxin taken is correct, and this method is easier.
Citrinin content of toxins is detected in the preserved red beancurd sample C of table 3
Embodiment above is only that the preferred embodiment of the present invention is described, and not the scope of the present invention is entered
Row is limited, on the premise of design spirit of the present invention is not departed from, technical side of this area ordinary skill technical staff to the present invention
In all variations and modifications that case is made, the protection domain that claims of the present invention determination all should be fallen into.
Claims (9)
1. a kind of method extracted and detect citrinin toxin in preserved red beancurd, it is characterised in that including step：
1) preserved red beancurd sample and methanol are mixed, reaction extracts citrinin toxin soiutions；Wherein preserved red beancurd sample and methanol
Mass volume ratio is 1g：(5-20mL)；
2) step 1) extract obtained citrinin toxin soiutions high performance liquid chromatography detection.
2. according to the method described in claim 1, it is characterised in that the methanol is hplc grade methanol.
3. method according to claim 2, it is characterised in that the methanol is hplc grade methanol, preserved red beancurd sample and first
The mass volume ratio of alcohol is 1g：5mL.
4. according to the method described in claim 1, it is characterised in that step 1), after preserved red beancurd sample is mixed with methanol, room temperature
Under with 100~300rpm, 30~120min of speed oscillation, then centrifuge, it is citrinin toxin soiutions to take supernatant.
5. method according to claim 4, it is characterised in that the rotating speed of the centrifugation is 7000~10000rpm,
The time of centrifugation is 8~15min.
6. the method according to any one of Claims 1 to 5, it is characterised in that step 2) in, the condition of high performance liquid chromatography
For：Chromatographic column：Agilent TC-C18,4.6 × 250mm, 5 μm；Acetonitrile/isopropanol/0.08mol/L phosphoric acid that mobile phase is is molten
Liquid, the volume ratio of acetonitrile/isopropanol/0.08mol/L phosphoric acid is 35：10：55.
7. the method according to any one of Claims 1 to 5, it is characterised in that step 2) in, examined with fluorescence detector
Survey, Detection wavelength is 331nm excitation wavelengths and 500nm launch wavelengths；Flow velocity is 1.0mL/min；40 DEG C of column temperature；The μ of sample size 50
L。
8. the method according to any one of Claims 1 to 5, it is characterised in that step 2) collect and citrinin toxin standard
The eluent at the consistent peak of product retention time, is quantitative determined using external standard method, obtains the citrinin poison in preserved red beancurd sample
Cellulose content, the retention time is front and rear 0.05min.
9. method according to claim 8, it is characterised in that be dissolved in hplc grade methanol with citrinin standard items, be configured to
The standard curve working solution of 0.01~10 μ g/g series concentrations.Using standard curve work of the high performance liquid chromatography to various concentrations
Make liquid progress HPLC quantitatively to detect, and abscissa is made with citrinin concentration, made with the peak area at 0.05min before and after retention time
Ordinate, carries out linear regression according to concentration and the relation of peak area, standard curve is drawn, for external standard method.
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| CN112098559A (en) * | 2020-09-22 | 2020-12-18 | 福州大学 | Method for detecting content of citrinin |
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Non-Patent Citations (5)
| Title |
|---|
| 熊勇华 等: "橙色红曲菌液体发酵产桔霉素特性的研究", 《食品科学》 * |
| 虞慧玲 等: "红曲桔霉素样品预处理的探讨", 《食品与发酵工业》 * |
| 许赣荣 等: "红曲霉桔霉素的检测方法及红曲霉产桔霉素的判别方法", 《微生物学通报》 * |
| 邹乐花 等: "橙色红曲菌As3. 4384 orf7 基因缺失株的构建及其功能分析", 《中国生物工程杂志》 * |
| 黄化成 等: "高效液相色谱法同时测定酱油中黄曲霉素B1、棕曲霉毒素A和桔霉素", 《色谱》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112098559A (en) * | 2020-09-22 | 2020-12-18 | 福州大学 | Method for detecting content of citrinin |
| CN112098559B (en) * | 2020-09-22 | 2021-12-28 | 福州大学 | Method for detecting content of citrinin |
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