CN114184776A - Silage aflatoxin detection kit and detection method - Google Patents

Silage aflatoxin detection kit and detection method Download PDF

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CN114184776A
CN114184776A CN202111522653.2A CN202111522653A CN114184776A CN 114184776 A CN114184776 A CN 114184776A CN 202111522653 A CN202111522653 A CN 202111522653A CN 114184776 A CN114184776 A CN 114184776A
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aflatoxin
silage
kit
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acetonitrile
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李旭业
尤海洋
董扬
王敏
张超
李莉
郭文凯
尹君伊
白长胜
张海红
杨淑萍
刘丽秋
刘秀玲
王佳
郭春晖
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    • G01N30/02—Column chromatography
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    • G01—MEASURING; TESTING
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    • G01N30/28—Control of physical parameters of the fluid carrier
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    • G01N30/28—Control of physical parameters of the fluid carrier
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    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2333/00—Assays involving biological materials from specific organisms or of a specific nature
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Abstract

The application provides a silage aflatoxin detection kit and a corresponding detection method. The kits and methods of the present application use 1:1:1 or 3:3:1 acetonitrile: water: the ether mixed solution is used as an extraction solvent to extract aflatoxin B1 in the silage, compared with the existing methanol aqueous solution, the extraction efficiency and the extraction stability are effectively improved, and the detection labor, time and reagent cost are effectively saved.

Description

Silage aflatoxin detection kit and detection method
Technical Field
The application belongs to the field of food and feed safety detection, and particularly provides an aflatoxin detection kit for silage and a corresponding detection method.
Background
Ensiling refers to a process of converting carbohydrates into organic acids mainly comprising lactic acid by anaerobic fermentation of lactic acid bacteria and the like attached to ensiling raw materials under a sealed condition, lowering the pH, and inhibiting the growth of harmful bacteria, thereby enabling the feed to be stored for a long time and optimizing the nutritional value thereof. Silage is one of the main sources of livestock feed in cold regions since ancient times, the silage mainly comprises corn, alfalfa, barley, oat, sorghum, milk vetch, beet, potato and the like, and the corn which is wide in planting, large in yield and convenient to operate is the main silage variety in the north of China.
Besides indexes such as sensory quality, pH, organic acid content, protein content and various fiber contents, the silage also needs to pay attention to an important safety index of aflatoxin, the speed of the aflatoxin is a necessary product in the fermentation process of the silage (the growth of microorganisms producing the aflatoxin cannot be completely inhibited by the existing methods), although the influence of the aflatoxin on the ruminant per se is small, the toxin can influence the digestion function of the ruminant on the one hand, and on the other hand, the aflatoxin in subsequent meat and milk products can exceed the standard. At present, food safety is increasingly emphasized, and accurate detection of aflatoxin is more and more important under the large background that standards are continuously improved.
The most common aflatoxin detection means in the practical operation of the food and feed industries is an ELISA kit, which is convenient to operate and does not need complex instruments; liquid chromatography and even mass spectrometry approaches may be used where more precise and stringent detection is required. In any method, the pretreatment of the sample/extraction of the aflatoxin is the basis of accurate detection, and for most food and agricultural product samples, the extraction rate of methanol, acetonitrile, trichloromethane and other solvents can reach more than 80% (methanol aqueous solution with the volume ratio of 1:1 or 8:2 recommended in GB17480-2008 and GB 30955-2014) and the accuracy is very good.
Disclosure of Invention
We find that a serious problem exists in the existing extraction/detection method in the practice of detecting the aflatoxin in the silage, and for samples with complex components and strong heterogeneity (different parts of the whole corn are fermented by a plurality of microorganisms for a long time), the existing methanol aqueous solution or chloroform solution has the problems of large fluctuation of extraction rate (reflected by obvious difference of detection values, even reaching more than 40%) and low extraction rate for some samples. After eliminating the problem of the detection equipment, we believe that the problem may be related to the presence of certain lipids in the silage, although the crude fat content of corn silage is typically only around 3% (no special treatment is required by the standard of GB 17480-2008), but the presence of these lipids, such as the encapsulation state, may have an effect on the aflatoxin release/dissolution process.
In order to solve the problems, various extraction methods and solvents are tried, and the fact that the extraction effect can be effectively improved after a proper amount of diethyl ether (AFB 1 is basically insoluble in diethyl ether) which is generally considered to be unsuitable for extracting aflatoxin B1 is added into the extraction solvent is found, so that the extraction rate is improved, and the stability of the extraction rate is further improved.
On one hand, the application provides a silage aflatoxin detection kit, which is characterized by comprising an extraction solvent consisting of more than two components of acetonitrile, water and diethyl ether.
Further, the aflatoxin is aflatoxin B1, and the silage is whole-plant corn silage.
Further, the kit also comprises an ELISA or liquid phase detection reagent.
Further, the extraction solvent consists of acetonitrile, water and diethyl ether.
Further, the extraction solvent comprises acetonitrile: water: the volume ratio of the ethyl ether is 1:1:1 or 3:3: 1.
Further, the extraction solvent comprises acetonitrile: water: the volume ratio of the diethyl ether was 3:3: 1.
In another aspect, the application provides a method for detecting aflatoxin B1 in silage, which is characterized in that the kit is used in the method.
Further, the method uses the extraction solvent in the kit to extract aflatoxin B1 in the sample.
Further, the method also comprises an ELISA or liquid phase detection step.
In another aspect, the present application provides acetonitrile in a volume ratio of 1:1:1 or 3:3: 1: water: application of diethyl ether mixed liquor in extraction of aflatoxin B1 in silage.
Detailed Description
The main experimental reagents and experimental methods are as follows:
the main apparatus is as follows:
chromatography apparatus and detector: agilent LC-1200 (with fluorescence detector);
a chromatographic column: agilent SB C-18 column (4.6 mm. times.250 mm);
an immunoaffinity column for aflatoxin purification: qingdao Purapang.
Aflatoxin B1 standard: xinyang Yaolai Biotechnology, Inc.;
methanol, acetonitrile, diethyl ether, chloroform, sodium hydroxide: shanghai test card;
ultrapure water: the applicant laboratory self-made;
aflatoxin B1 detection kit: ELISA method, Shanghai healthy color Biotech Ltd;
whole corn silage product: the applicant self-prepares in factories, selects a plurality of batches of samples with good fermentation state, and detects (a detection mode commonly used in factories) through the kit, wherein the content of aflatoxin B1 is lower than 5 mug/kg;
other unexhausted reagents are of the general domestic variety.
The basic extraction method comprises the following steps:
detection by an ELISA kit: crushing and uniformly mixing the sample, weighing 5g of the sample, adding the weighed sample into a 50mL centrifuge tube, adding 10mL of the extracting solution, shaking and mixing for 5min, and filtering (taking the middle-stage filtrate as a detection sample);
liquid phase detection: after crushing and uniformly mixing the samples, weighing 20g, adding the weighed 20g and 4g of NaOH into a 250mL triangular flask, adding 100mL of extracting solution, stirring and mixing for 2min, and filtering twice; purifying with immunoaffinity column, eluting with methanol, and collecting the sample.
The basic detection method comprises the following steps:
detection by an ELISA kit: except for the extract fraction, the procedure was as indicated in the kit.
Liquid phase detection: mobile phase: water-acetonitrile-methanol (60: 5: 35); flow rate: 1.0 mL/min; sample introduction amount: 30 mu L of the solution; column temperature: 30 ℃ and is detected and calculated by referring to GB 30955-2014.
EXAMPLE 1 stability of the assays for different samples
Selecting 50 parts of samples from different positions of 5 batches of silage products (10 parts of samples are selected for each batch); using methanol aqueous solution with a volume ratio of 1:1 as an extraction solvent, detecting the aflatoxin B1 content by an ELISA method for 5 times (completing 5 operations from the beginning of the extraction step), and finding that 12 samples have obvious difference between the highest value and the lowest value (the highest value is more than 1.2 times of the lowest value), wherein 4 samples have the most obvious difference, and the detection results of the 4 samples are shown in Table 1:
TABLE 1 results measurement of aflatoxin content of unstabilized samples (AFB 1 content, μ g/kg)
Figure 148190DEST_PATH_IMAGE002
The results show that for some silage samples, the existing methanol aqueous solution as an extraction solvent has obvious unstable detection results, and whether the occurrence rate (about 22%) or the deviation degree (the highest value reaches about 1.5 times of the lowest value) completely possibly influences the evaluation result of the toxicity of the silage product.
Example 2 stability of assays with different extraction solvents
The effect of 5 improved extraction solvents was verified using unstable samples 2, 3 in table 1 (5 shown are representative combinations, more preliminary experimental formulations are not shown):
TABLE 2 examination of the different extraction solvents (unstable sample 2, AFB1 content,. mu.g/kg)
Figure 376915DEST_PATH_IMAGE004
TABLE 3 examination results of different extraction solvents (unstable sample 3, AFB1 content, μ g/kg)
Figure 156652DEST_PATH_IMAGE006
The result shows that the acetonitrile-water-ethyl ether with the volume ratio of 3:3:1 or 1:1:1 can effectively dissolve/release AFB1 in the silage sample, and the stability of the detection result is improved.
Subsequent practical application also proves that the extraction of acetonitrile-water-ether with the volume ratio of 3:3:1 can effectively reduce the occurrence of unstable detection. In the past production experience, the proportion of samples needing repeated detection (the highest value in 3 times of detection is more than 1.2 times of the lowest value) is about 10-20%; this ratio dropped to less than 2% after using 3:3:1 acetonitrile-water-ether as the extraction solvent. Effectively saving the detection labor, time and reagent cost.
Example 3 recovery assay with spiking
Selecting a sample crushed material (the AFB1 is lower than 0.3 mu g/kg according to the prediction of the kit instruction) of which the aflatoxin B1 is not detected by an ELISA method, adding the aflatoxin B1 standard substance according to the amount of 5 mu g/kg, 10 mu g/kg and 20 mu g/kg, and uniformly mixing. And (3) detecting the recovery rate of the added standard by using a liquid phase detection method by using methanol aqueous solution and acetonitrile-water-ether in a volume ratio of 8:2 to 3:1 or 1:1:1 as extraction solvents.
The results are shown in the following table:
TABLE 4 recovery on spiking of different concentrations and extraction reagents (triplicate average,%)
5μg/kg 10μg/kg 20μg/kg
8:2 aqueous methanol solution 75.3 78.4 86.2
Acetonitrile: water: ether =1:1 76.4 77.6 85.9
Acetonitrile: water: ether =3:3:1 80.5 83.2 87.1
The result shows that the 3:3:1 acetonitrile-water-ethyl ether can achieve better extraction rate than the existing commonly used 8:2 methanol aqueous solution, and particularly the improvement is more obvious under the condition of lower aflatoxin B1 content, which is very helpful for improving the accuracy of actual detection (the content of aflatoxin B1 in silage is 20 mu g/kg or even less than 10 mu g/kg in most cases).
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And such obvious variations or modifications which fall within the spirit of the invention are intended to be covered by the scope of the present invention.

Claims (10)

1. The silage aflatoxin detection kit is characterized by comprising an extraction solvent consisting of more than two components of acetonitrile, water and diethyl ether.
2. The kit of claim 1, wherein the aflatoxin is aflatoxin B1 and the silage is whole corn silage.
3. The kit according to claim 1 or 2, wherein the kit further comprises a reagent for ELISA or liquid phase detection.
4. The kit according to any one of claims 1 to 3, wherein the extraction solvent consists of acetonitrile, water, diethyl ether.
5. The kit of claim 4, wherein the extraction solvent comprises acetonitrile: water: the volume ratio of the ethyl ether is 1:1:1 or 3:3: 1.
6. The kit of claim 5, wherein the extraction solvent comprises acetonitrile: water: the volume ratio of the diethyl ether was 3:3: 1.
7. A method for detecting aflatoxin B1 in whole corn silage, wherein the kit of any one of claims 1-6 is used in the method.
8. The method according to claim 7, wherein the aflatoxin B1 in the sample is extracted in the method using the extraction solvent in the kit according to any one of claims 1-6.
9. The method of claim 7 or 8, wherein the method further comprises an ELISA or liquid phase detection step.
10. Acetonitrile in a volume ratio of 1:1:1 or 3:3: 1: water: the application of the ether mixed solution in extracting aflatoxin B1 in whole-plant corn silage.
CN202111522653.2A 2021-12-14 2021-12-14 Silage aflatoxin detection kit and detection method Pending CN114184776A (en)

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