CN110646268A - Pretreatment method for detecting inorganic arsenic in food - Google Patents
Pretreatment method for detecting inorganic arsenic in food Download PDFInfo
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- CN110646268A CN110646268A CN201911052051.8A CN201911052051A CN110646268A CN 110646268 A CN110646268 A CN 110646268A CN 201911052051 A CN201911052051 A CN 201911052051A CN 110646268 A CN110646268 A CN 110646268A
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- food
- inorganic arsenic
- pretreatment method
- centrifugal treatment
- detecting inorganic
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
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- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Biomedical Technology (AREA)
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- Sampling And Sample Adjustment (AREA)
Abstract
The application discloses a pretreatment method for detecting inorganic arsenic in food, which comprises the following steps: 1) sampling; 2) and (3) extracting: placing the sample solution after standing into a plastic flask with magnetic stirring, and heating the plastic flask in a water bath under the condition of stirring; 3) carrying out primary centrifugal treatment; 4) performing secondary centrifugal treatment; 5) and filtering and purifying. The pretreatment method for detecting inorganic arsenic in food is simple to operate, stirring is carried out while heating, the transfer of inorganic arsenic is accelerated, the time for pretreatment of samples is shortened, and the efficiency is improved.
Description
Technical Field
The invention relates to the technical field of rapid food detection, in particular to a pretreatment method for detecting inorganic arsenic in food.
Background
Arsenic is a metalloid element commonly existing in nature and has wide application in industrial and agricultural production. Arsenic has different forms and valence state distributions, and mainly comprises inorganic forms and organic forms, wherein the toxicity of the inorganic form of arsenic is far higher than that of organic arsenic, so that the detection of the inorganic arsenic in food has important significance for food quality control. According to the requirements of the national standard GB5009.11-2014 for measuring total arsenic and inorganic arsenic in food safety national standard food, the pretreatment process for detecting the inorganic arsenic in aquatic animals, infant cereals and canned auxiliary food is to thermally extract at 90 ℃ for 2.5h and shake for 1min every 0.5h, and the thermal extraction time is long, so that the detection efficiency is low.
Disclosure of Invention
The present invention aims to solve at least one of the problems of the prior art or at least to provide a commercial choice. Therefore, the invention aims to provide a pretreatment method for detecting inorganic arsenic in food.
In order to achieve the purpose, the invention provides the following technical scheme:
the embodiment of the application discloses a pretreatment method for detecting inorganic arsenic in food, which comprises the following steps: 1) and sampling: weighing 1.0g of food sample in a 50mL plastic centrifuge tube, adding 0.15mol/L nitric acid solution, and standing overnight; 2) and (3) extracting: placing the sample solution after standing into a plastic flask with magnetic stirring, and heating and extracting the plastic flask in a water bath under the condition of stirring; 3) and primary centrifugal treatment: taking out the extracted patterns, cooling to room temperature, and placing the patterns into a centrifuge for primary centrifugation; 4) and secondary centrifugal treatment: adding 5mL of n-hexane into 5mL of supernatant, shaking for 1min, centrifuging for the second time, removing the upper n-hexane layer, and repeating the process once; 5) and filtering and purifying: absorbing the lower clear liquid, filtering with 0.45 μm organic filter membrane and filtering18Purifying with small column to obtain sample.
Preferably, in the pretreatment method for detecting inorganic arsenic in food, the nitric acid solution is added in the step 1) in a volume of 10-20 mL.
Preferably, in the pretreatment method for detecting inorganic arsenic in food, the sample solution heated in the water bath in step 2) is kept at 90 ℃ for 40-60 min.
Preferably, in the pretreatment method for detecting inorganic arsenic in food, the parameters of the primary centrifugation treatment and the secondary centrifugation treatment are 8000r/min and 15min of centrifugation.
Compared with the prior art, the invention has the advantages that: the pretreatment method for detecting inorganic arsenic in food is simple to operate, stirring is carried out while heating, the transfer of inorganic arsenic is accelerated, the time for pretreatment of samples is shortened, and the efficiency is improved.
Detailed Description
The invention is further illustrated by the following examples: the invention will be better understood from the following examples. However, those skilled in the art will readily appreciate that the specific material ratios, process conditions and results thereof described in the examples are illustrative only and should not be taken as limiting the invention as detailed in the claims.
Example one
The pretreatment method for detecting inorganic arsenic in food in the specific embodiment of the invention comprises the following steps: 1) and sampling: weighing 1.0g of rice sample in a 50mL plastic centrifuge tube, adding 20mL0.15mol/L nitric acid solution, and standing overnight; 2) and (3) extracting: placing the sample solution after standing into a plastic flask with magnetic stirring, heating the plastic flask to 90 ℃ in a water bath under the condition of stirring, and extracting for 40 min; 3) and primary centrifugal treatment: taking out the extracted pattern, cooling to room temperature, and centrifuging for 15min at 8000 r/min; 4) and secondary centrifugal treatment: adding 5mL of n-hexane into 5mL of supernatant, shaking for 1min, centrifuging at 8000r/min for 15min, discarding the upper n-hexane layer, and repeating the process once; 5) and filtering and purifying: absorbing the lower clear liquid, filtering with 0.45 μm organic filter membrane and filtering18Purifying with small column to obtain sample.
Example one
The pretreatment method for detecting inorganic arsenic in food in the specific embodiment of the invention comprises the following steps: 1) and sampling: weighing 1.0g of infant auxiliary food sample into a 50mL plastic centrifuge tube, adding 10mL0.15mol/L nitric acid solution, and standing overnight; 2) and (3) extracting: placing the sample solution after standing into a plastic flask with magnetic stirring, heating the plastic flask to 90 ℃ in a water bath under the condition of stirring, and extracting for 60 min; 3) and primary centrifugal treatment: taking out the extracted pattern, cooling to room temperature, and centrifuging for 15min at 8000 r/min; 4) and secondary centrifugal treatment: adding 5mL of n-hexane into 5mL of supernatant, shaking for 1min, centrifuging at 8000r/min for 15min, discarding the upper n-hexane layer, and repeating the process once; 5) and filtering and purifying: absorbing the lower clear liquid, filtering with 0.45 μm organic filter membrane and filtering18Purifying with small column to obtain sample.
In conclusion, the pretreatment method for detecting inorganic arsenic in food is simple to operate, stirring is carried out while heating, the transfer of inorganic arsenic is accelerated, the sample pretreatment time is shortened, and the efficiency is improved.
It should be noted that, in order to avoid obscuring the present invention with unnecessary details, only the structures and/or processing steps closely related to the scheme according to the present invention are described in the embodiments, and other details not closely related to the present invention are omitted.
Finally, it should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Claims (4)
1. A pretreatment method for detecting inorganic arsenic in food is characterized in that: the method comprises the following steps: 1) and sampling: weighing 1.0g of food sample in a 50mL plastic centrifuge tube, adding 0.15mol/L nitric acid solution, and standing overnight; 2) and (3) extracting: placing the sample solution after standing into a plastic flask with magnetic stirring, and heating and extracting the plastic flask in a water bath under the condition of stirring; 3) and primary centrifugal treatment: taking out the extracted patterns, cooling to room temperature, and placing the patterns into a centrifuge for primary centrifugation; 4) and secondary centrifugal treatment: adding 5mL of n-hexane into 5mL of supernatant, shaking for 1min, centrifuging for the second time, removing the upper n-hexane layer, and repeating the process once; 5) and filtering and purifying: absorbing the lower clear liquid, filtering with 0.45 μm organic filter membrane and filtering18Purifying with small column to obtain sample.
2. The pretreatment method for detecting inorganic arsenic in food according to claim 1, wherein: the volume of the nitric acid solution added in the step 1) is 10-20 mL.
3. The pretreatment method for detecting inorganic arsenic in food according to claim 1, wherein: the sample solution heated by the water bath in the step 2) is kept at 90 ℃ for 40-60 min.
4. The pretreatment method for detecting inorganic arsenic in food according to claim 1, wherein: the parameters of the primary centrifugal treatment and the secondary centrifugal treatment are 8000r/min and 15min of centrifugation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911052051.8A CN110646268A (en) | 2019-10-31 | 2019-10-31 | Pretreatment method for detecting inorganic arsenic in food |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911052051.8A CN110646268A (en) | 2019-10-31 | 2019-10-31 | Pretreatment method for detecting inorganic arsenic in food |
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| Publication Number | Publication Date |
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| CN110646268A true CN110646268A (en) | 2020-01-03 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911052051.8A Pending CN110646268A (en) | 2019-10-31 | 2019-10-31 | Pretreatment method for detecting inorganic arsenic in food |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105533400A (en) * | 2015-12-16 | 2016-05-04 | 胡彩军 | Hizikia fusifarme arsenic removing method |
| CN110308229A (en) * | 2019-08-13 | 2019-10-08 | 深圳凯吉星农产品检测认证有限公司 | A method of abio-arsenic residues in measurement seaweed based article |
-
2019
- 2019-10-31 CN CN201911052051.8A patent/CN110646268A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105533400A (en) * | 2015-12-16 | 2016-05-04 | 胡彩军 | Hizikia fusifarme arsenic removing method |
| CN110308229A (en) * | 2019-08-13 | 2019-10-08 | 深圳凯吉星农产品检测认证有限公司 | A method of abio-arsenic residues in measurement seaweed based article |
Non-Patent Citations (3)
| Title |
|---|
| 王秋云: "食品中无机砷的测定分析", 《科技经济导刊》 * |
| 赵海峰等: "悬浮液进样 氢化物发生原子荧光光谱法测定土壤中砷的方法研究", 《农业与技术》 * |
| 边疆等: "氢化物发生原子荧光法测定硅藻土中砷", 《中国卫生检验杂志》 * |
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Application publication date: 20200103 |