CN104502481A - Method for detecting vomitoxin and zearalenone in grains and feeds - Google Patents
Method for detecting vomitoxin and zearalenone in grains and feeds Download PDFInfo
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- CN104502481A CN104502481A CN201410835645.7A CN201410835645A CN104502481A CN 104502481 A CN104502481 A CN 104502481A CN 201410835645 A CN201410835645 A CN 201410835645A CN 104502481 A CN104502481 A CN 104502481A
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Abstract
The invention discloses a method for detecting vomitoxin and zearalenone in grains and feeds. The method comprises the following steps: A, adding 25g of a to-be-detected sample into a 250ml conical flask; B, adding 100ml of an extracting solution into the conical flask, and shaking the conical flask on a shaker for 20 minutes to obtain a mixed solution; C, adding 8ml of the mixed solution into a glass test tube, adding 80mul of acetic acid into the test tube, and performing column purification by virtue of a multifunctional purification column to obtain a purification solution; D, adding 250 microlitres of the purification solution into a container, adding deionized water containing 0.05 percent of acetic acid into the container for making up to volume to 1ml, thereby obtaining a test sample; and E, extracting the solution from the test sample, detecting by utilizing a multi-reaction detection mode of a liquid chromatography-tandem mass spectrometer, thereby obtaining data of the vomitoxin and the zearalenone respectively. According to the method, the operation steps have the time/labor-saving effect, the production and processing cost is reduced, and the detection result is relatively accurate and sensitive.
Description
Technical field
The present invention relates to and measure vomiting mycin and the application of zearalenone method, particularly a kind ofly detect in Fodder and food the method for vomitting mycin and zearalenone.
Background technology
At present, often need to measure respectively to the assay method vomitting mycin and zearalenone content in Fodder and food, and all need very loaded down with trivial details step, and need to use a large amount of assisted solution reagent and solid sample, so not only make operation steps become to waste time and energy, also because measuring and add a large amount of reagent, sample and improve the cost of production and processing respectively, meanwhile, also there is measurement result out of true, the defect such as insensitive in this assay method.
Summary of the invention
For solving Problems existing in above-mentioned background technology, the object of the present invention is to provide and a kind ofly detect in Fodder and food the method for vomitting mycin and zearalenone, operation steps is not only made to become time saving and energy saving to reach, also reduce the cost of production and processing, and measurement result more accurately, sensitiveer object.
For achieving the above object, technical scheme of the present invention is as follows:
Detect in Fodder and food a method of vomitting mycin and zearalenone, comprise the following steps:
A, get 25g testing sample in the conical flask of 250ml, and record gravimetric value;
B, in above-mentioned conical flask, add 100ml extract (ratio of first alcohol and water is 84:16), conical flask to be placed on rocker jolting 20 minutes, then through Filter paper filtering, to obtain mixed solution;
C, get above-mentioned mixed solution 8ml in glass test tube, and to adding 80 μ l acetic acid in it, through Multifunctional cleanup column to its column purification, be purified liquid;
D, get the above-mentioned scavenging solution of 250 μ l in container, and be settled to 1ml to the deionized water added containing 0.05% acetic acid in this container, obtain test sample book;
E, above-mentioned test sample book is extracted solution, many reaction detection pattern of recycling Liquid Chromatography-Tandem Mass Spectrometry instrument detects, and obtains the data of vomitting mycin and zearalenone respectively.
Preferably, the quantitative sense channel of described vomitoxin :-295.0/265.0, qualitative detection passage :-295.0/138.0.
Preferably, the quantitative sense channel of described zearalenone :-317.0/174.8, qualitative detection passage :-317.0/131.0.
Pass through technique scheme, provided by the inventionly a kind ofly detect in Fodder and food the method for vomitting mycin and zearalenone, vomiting mycin and zearalenone Simultaneously test not only can be made by this assay method, also can eliminate the step of a lot of operation, decrease the use of assisted solution reagent and solid sample, operation steps is not only made to become time saving and energy saving, also because avoiding measuring respectively and decreasing reagent, sample and reduce the cost of production and processing, this assay method is owing to have employed more accurate proportion relation, make its testing result more accurate, sensitiveer.
Embodiment
Be clearly and completely described to the technical scheme in the embodiment of the present invention below.
Provided by the inventionly a kind ofly detect in Fodder and food the method for vomitting mycin and zearalenone, comprise the following steps:
A, get 25g testing sample in the conical flask of 250ml, and record gravimetric value;
B, in above-mentioned conical flask, add 100ml extract (ratio of first alcohol and water is 84:16), conical flask to be placed on rocker jolting 20 minutes, then through Filter paper filtering, to obtain mixed solution;
C, get above-mentioned mixed solution 8ml in glass test tube, and to adding 80 μ l acetic acid in it, through Multifunctional cleanup column to its column purification, be purified liquid;
D, get the above-mentioned scavenging solution of 250 μ l in container, and be settled to 1ml to the deionized water added containing 0.05% acetic acid in this container, obtain test sample book;
E, above-mentioned test sample book is extracted solution, many reaction detection pattern of recycling Liquid Chromatography-Tandem Mass Spectrometry instrument detects, obtain the data of vomitting mycin and zearalenone respectively, the quantitative sense channel of vomitoxin :-295.0/265.0, qualitative detection passage :-295.0/138.0; The quantitative sense channel of zearalenone :-317.0/174.8, qualitative detection passage :-317.0/131.0.
Disclosed by the inventionly a kind ofly detect in Fodder and food the method for vomitting mycin and zearalenone, vomiting mycin and zearalenone Simultaneously test not only can be made by this assay method, also can eliminate the step of a lot of operation, decrease the use of assisted solution reagent and solid sample, operation steps is not only made to become time saving and energy saving, also because avoiding measuring respectively and decrease reagent, sample and reduce the cost of production and processing, this assay method owing to have employed more accurate proportion relation, make its testing result more accurately, sensitiveer.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (3)
1. detect in Fodder and food a method of vomitting mycin and zearalenone, it is characterized in that, comprise the following steps:
A, get 25g testing sample in the conical flask of 250ml, and record gravimetric value;
B, in above-mentioned conical flask, add 100ml extract (ratio of first alcohol and water is 84:16), conical flask to be placed on rocker jolting 20 minutes, then through Filter paper filtering, to obtain mixed solution;
C, get above-mentioned mixed solution 8ml in glass test tube, and to adding 80 μ l acetic acid in it, through Multifunctional cleanup column to its column purification, be purified liquid;
D, get the above-mentioned scavenging solution of 250 μ l in container, and be settled to 1ml to the deionized water added containing 0.05% acetic acid in this container, obtain test sample book;
E, above-mentioned test sample book is extracted solution, many reaction detection pattern of recycling Liquid Chromatography-Tandem Mass Spectrometry instrument detects, and obtains the data of vomitting mycin and zearalenone respectively.
2. according to claim 1ly a kind ofly detect in Fodder and food the method for vomitting mycin and zearalenone, it is characterized in that, the quantitative sense channel of described vomitoxin :-295.0/265.0, qualitative detection passage :-295.0/138.0.
3. according to claim 1ly a kind ofly detect in Fodder and food the method for vomitting mycin and zearalenone, it is characterized in that, the quantitative sense channel of described zearalenone :-317.0/174.8, qualitative detection passage :-317.0/131.0.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109696462A (en) * | 2019-01-17 | 2019-04-30 | 重庆医科大学 | A kind of electrochemical sensor preparation method detected for zearalenone in grain or feed |
CN110007029A (en) * | 2019-04-28 | 2019-07-12 | 江南大学 | A kind of method of vomitoxin in detection wheat |
CN111707753A (en) * | 2020-06-24 | 2020-09-25 | 安徽农业大学 | Detection method of wheat scab grain ZEN toxin |
-
2014
- 2014-12-29 CN CN201410835645.7A patent/CN104502481A/en active Pending
Non-Patent Citations (7)
Title |
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MICHAEL SULYOK ET AL.: "Development and validation of a liquid chromatography/tandem mass spectrometric method for the determination of 39 mycotoxins in wheat and maize", 《RAPID COMMUNICATIONS IN MASS SPECTROMETRY》 * |
NICK BYRD ET AL.: "《应用报告 食品检测和农业》", 2 February 2012 * |
SZABOLCS B. TO´TH ET AL.: "Analysis of Deoxynivalenol, Nivalenol, Zearalenone in Food by LC–APCI–MS", 《CHROMATOGRAPHIA》 * |
WWW.UNITEDCHEM.COM: "《UCT》", 30 September 2014 * |
任一平 等: "液质联用法检测食品和饲料中的多组分霉菌毒素的残留", 《浙江省第三届分析测试学术报告会》 * |
刘柱 等: "多功能柱净化-柱后光化学衍生-高效液相色谱法同时检测玉米和花生中9种真菌毒素", 《分析科学学报》 * |
朱群英 等: "液质联用同位素内标法同时测定小麦粉中7种真菌毒素", 《现代预防医学》 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109696462A (en) * | 2019-01-17 | 2019-04-30 | 重庆医科大学 | A kind of electrochemical sensor preparation method detected for zearalenone in grain or feed |
CN110007029A (en) * | 2019-04-28 | 2019-07-12 | 江南大学 | A kind of method of vomitoxin in detection wheat |
CN111707753A (en) * | 2020-06-24 | 2020-09-25 | 安徽农业大学 | Detection method of wheat scab grain ZEN toxin |
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Application publication date: 20150408 |