CN110967412A - Pretreatment method for detecting food containing mycotoxin based on accelerated solvent extraction - Google Patents
Pretreatment method for detecting food containing mycotoxin based on accelerated solvent extraction Download PDFInfo
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- CN110967412A CN110967412A CN201811137416.2A CN201811137416A CN110967412A CN 110967412 A CN110967412 A CN 110967412A CN 201811137416 A CN201811137416 A CN 201811137416A CN 110967412 A CN110967412 A CN 110967412A
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- food
- solvent extraction
- accelerated solvent
- pretreatment method
- extracting solution
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- 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
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- 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
-
- 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
- G01N2030/062—Preparation extracting sample from raw material
Abstract
The invention discloses a pretreatment method for detecting food containing mycotoxin based on accelerated solvent extraction, which comprises the following steps: firstly, crushing solid food, or concentrating liquid food to be viscous, weighing 0.5g of the liquid food, uniformly mixing the liquid food with a proper amount of diatomite, and filling the mixture into an extraction pool of 11mL of an accelerated solvent extraction instrument. The accelerated solvent extraction conditions were: solvent: acetonitrile-water (80: 20, V: V), time: 5 minutes, temperature: 100 ℃, cycle number: 1 time. Transferring the collected extracting solution into a round-bottom flask for rotary steaming; redissolved with acetonitrile-water (80: 20, V: V) to 3 mL. After centrifugal precipitation, the supernatant clear liquid is sucked and passes through an Shimadzu VRA-1 column, the effluent clear liquid is collected and passes through a 0.22 mu m filter membrane.
Description
Technical Field
The invention relates to the field of food safety, in particular to a pretreatment method for detecting food containing mycotoxin based on accelerated solvent extraction.
Background
Compared with the traditional liquid-liquid extraction, Soxhlet extraction and the like, the accelerated solvent extraction pretreatment technology has the characteristics of high automation degree, less solvent consumption and short time consumption, and greatly improves the analysis efficiency. The food has complex and various matrixes which can be roughly divided into solid food and liquid food, the content of the mycotoxin which is a common pollutant in the food is often a trace amount, and the mycotoxin is subjected to pretreatment such as extraction, purification and the like, is important for subsequent analysis and is a limiting factor of the analysis speed. Therefore, development of a sample pretreatment technique based on an efficient accelerated solvent extraction technique is urgently required.
Disclosure of Invention
The invention aims to overcome the defects of the traditional fussy pretreatment method, adopts an accelerated solvent extraction method with high automation degree, small solvent consumption and short time consumption, greatly improves the efficiency of food analysis, and can be used as a pretreatment method for analyzing food polluted by mycotoxin.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
1) pulverizing solid food, or concentrating liquid food to viscous; weighing 3g of diatomite, uniformly mixing with a proper amount of diatomite, and filling an 11mL extraction pool;
2) the accelerated solvent extraction conditions for step 1) are: solvent acetonitrile-water (80: 20, V: V), time: 5 minutes, temperature: 100 ℃, cycle number: 1 time;
3) transferring the extracting solution collected in the step 2) into a round-bottom flask for rotary evaporation until the extracting solution is dry;
4) redissolving the acetonitrile-water (80: 20, V: V) solution in the step 3) to a constant volume of 3 mL.
5) And (4) after centrifugal precipitation in the step 4), sucking the supernatant clarified liquid, passing the supernatant clarified liquid through an SPE small column, collecting effluent, and passing the effluent through a 0.22 mu m filter membrane to obtain an extracting solution.
Step 1) the solid food: such as grains and products thereof, vegetables and fruits with low water content, coffee powder, tea powder, etc. The liquid food is: such as wine, milk, grease, fruit juice, etc., are all suitable for the method.
The extracting solution in the step 5) can be directly subjected to high performance liquid chromatography or high performance liquid chromatography-mass spectrometry combined analysis.
The invention has the advantages and beneficial effects that:
the invention adopts an accelerated solvent extraction method with high automation degree, less solvent consumption and short time consumption, greatly improves the efficiency of food analysis, and can be used as a pretreatment method for analyzing food polluted by mycotoxin.
Detailed Description
Example 1
A pretreatment method for detecting food containing mycotoxin based on accelerated solvent extraction comprises the following five steps:
firstly, rice is crushed, 3g of the crushed rice is weighed and mixed with a proper amount of diatomite uniformly, and then an 11mL extraction pool is filled with the mixture. Secondly, carrying out accelerated solvent extraction under the following extraction conditions: solvent acetonitrile-water (80: 20, V: V), time: 5 minutes, temperature: 100 ℃, cycle number: 1 time. And thirdly, transferring the collected extracting solution into a round-bottom flask for rotary evaporation till the extracting solution is dry. And fourthly, redissolving by using acetonitrile-water (80: 20, V: V) solution to reach 3 mL. And fifthly, after centrifugal precipitation, sucking the supernatant clarified liquid to pass through an SPE small column, collecting the effluent liquid and passing through a 0.22 mu m filter membrane to obtain an extracting solution, and then carrying out subsequent analysis and identification.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and are intended to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and thus the protection scope of the present invention is not limited thereby. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (3)
1. A pretreatment method for detecting food containing mycotoxin based on accelerated solvent extraction is characterized in that:
1) pulverizing solid food, or concentrating liquid food to viscous; weighing 3g of diatomite, uniformly mixing with a proper amount of diatomite, and filling an 11mL extraction pool;
2) the accelerated solvent extraction conditions for step 1) are: solvent: acetonitrile-water (80: 20, V: V), time: 5 minutes, temperature: 100 ℃, cycle number: 1 time;
3) transferring the extracting solution collected in the step 2) into a round-bottom flask for rotary evaporation until the extracting solution is dry;
4) redissolving the acetonitrile-water (80: 20, V: V) solution in the step 3) to a constant volume of 3 mL.
5) And (4) after centrifugal precipitation in the step 4), sucking the supernatant clarified liquid, passing the supernatant clarified liquid through an SPE small column, collecting effluent, and passing the effluent through a 0.22 mu m filter membrane to obtain an extracting solution.
2. The accelerated solvent extraction based pretreatment method for detection of mycotoxin-containing food product of claim 1, wherein: step 1) the solid food: such as grains and their products, vegetables and fruits with low water content, coffee powder, tea powder, etc.; the liquid food is: such as wine, milk, grease, fruit juice, etc., are all suitable for the method.
3. The accelerated solvent extraction based pretreatment method for detection of mycotoxin-containing food product of claim 1, wherein: the extracting solution in the step 5) can be directly subjected to high performance liquid chromatography or high performance liquid chromatography-mass spectrometry combined analysis.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811137416.2A CN110967412A (en) | 2018-09-28 | 2018-09-28 | Pretreatment method for detecting food containing mycotoxin based on accelerated solvent extraction |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811137416.2A CN110967412A (en) | 2018-09-28 | 2018-09-28 | Pretreatment method for detecting food containing mycotoxin based on accelerated solvent extraction |
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| CN110967412A true CN110967412A (en) | 2020-04-07 |
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| CN201811137416.2A Pending CN110967412A (en) | 2018-09-28 | 2018-09-28 | Pretreatment method for detecting food containing mycotoxin based on accelerated solvent extraction |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002023168A2 (en) * | 2000-09-12 | 2002-03-21 | Ut-Battelle, Llc | Bioluminescent bioreporter integrated circuit detection methods |
| WO2013021100A1 (en) * | 2011-08-08 | 2013-02-14 | Thermo Fisher Scientific Oy | Method and apparatus for automated analysis |
| CN106093253A (en) * | 2016-05-27 | 2016-11-09 | 国家烟草质量监督检验中心 | The assay method of benzo [a] pyrene in the sample-pretreating method measuring benzo in cigarette smoke [a] pyrene and cigarette smoke |
-
2018
- 2018-09-28 CN CN201811137416.2A patent/CN110967412A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002023168A2 (en) * | 2000-09-12 | 2002-03-21 | Ut-Battelle, Llc | Bioluminescent bioreporter integrated circuit detection methods |
| WO2013021100A1 (en) * | 2011-08-08 | 2013-02-14 | Thermo Fisher Scientific Oy | Method and apparatus for automated analysis |
| CN106093253A (en) * | 2016-05-27 | 2016-11-09 | 国家烟草质量监督检验中心 | The assay method of benzo [a] pyrene in the sample-pretreating method measuring benzo in cigarette smoke [a] pyrene and cigarette smoke |
Non-Patent Citations (3)
| Title |
|---|
| 曹晓琴等: "高效液相色谱-串联质谱法测定多种食品和饲料中的胶霉毒素", 《食品与发酵工业》 * |
| 李梅等: "高效液相色谱串联质谱法测定食品中的10种真菌毒素", 《国际药学研究杂志》 * |
| 欧小群 等: "加速溶剂萃取技术在食品安全检测中的应用", 《中国食品学报》 * |
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