CN110361249A - A method of by four kinds of trace arsenic in rice kernels, cadmium, manganese and zinc element extractions into solution - Google Patents
A method of by four kinds of trace arsenic in rice kernels, cadmium, manganese and zinc element extractions into solution Download PDFInfo
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- CN110361249A CN110361249A CN201910681423.7A CN201910681423A CN110361249A CN 110361249 A CN110361249 A CN 110361249A CN 201910681423 A CN201910681423 A CN 201910681423A CN 110361249 A CN110361249 A CN 110361249A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0261—Solvent extraction of solids comprising vibrating mechanisms, e.g. mechanical, acoustical
- B01D11/0265—Applying ultrasound
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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
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- G01—MEASURING; TESTING
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- 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
- G01N1/40—Concentrating 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
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- G01N1/40—Concentrating 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
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- G01N1/4077—Concentrating samples by other techniques involving separation of suspended solids
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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
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
- G01N2001/4061—Solvent extraction
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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
- G01N1/40—Concentrating samples
- G01N1/4077—Concentrating samples by other techniques involving separation of suspended solids
- G01N2001/4094—Concentrating samples by other techniques involving separation of suspended solids using ultrasound
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Abstract
The present invention provides a kind of methods by trace arsenic in rice kernels, four kinds of cadmium, manganese and zinc element extractions into solution, belong to element analysis technology field.The present invention joined complexing agent ethylenediamine tetra-acetic acid (Ethylenediaminetetraacetic acid, EDTA), improve the rate of recovery of heavy metal element while being digested using pancreatin to rice.In addition, the present invention carries out a pickling to the substrate after enzymatic hydrolysis, to further improve the rate of recovery of element.Method of the invention can be extracted in solution in 20 minutes by trace arsenic in rice kernels, cadmium, manganese, zinc are quantitative, compared to the pretreatment technology of traditional rice elemental analysis, significantly shorten the processing time, avoid the use of strong oxidizer, reduce strong acid usage amount and energy consumption, compared to other zymolysis techniques, quantitatively extracted while realizing multielement in rice for the first time.
Description
Technical field
The present invention relates to element analysis technology field more particularly to a kind of four kinds of trace arsenic in rice kernels, cadmium, manganese and zinc elements are mentioned
Get the method in solution.
Background technique
The population of global nearly half is using rice as staple food.The edible safety of rice has become the hot spot of concern.Rice
The harmful elements such as arsenic (As), cadmium (Cd) in meeting enrichment environment, can generate the diseases such as nervous breakdown and osteomalacia after people is edible.This
Outside, the Excess free enthalpy of the human essential elements such as manganese (Mn) and zinc (Zn) can also cause disease in rice.Therefore multielement in rice
It analyzes particularly significant to ensuring food safety.
The core of multielement analysis is quantitatively to extract each element in rice in solution in rice.Currently used side
Method includes dry ashing method, wet digestion method and Microwave Digestion；Dry ashing method is to be made organic destruction by high temperature sintering
Organics dehydration, charing, decomposition, oxidation, calcination is ashed in high-temperature electric resistance furnace；Wet digestion is by oxidizing acid and oxidation
Agent aoxidizes organic matter in the case where heating heating condition, is hydrolyzed, achieved the purpose that inorganization；Microwave Digestion refers to utilization
Digestion solution (usually containing strong acid and strong oxidizer) and sample in microwave heating closed container, to make under high-temperature and high-pressure conditions
The rapidly-soluble method of sample.
The shortcomings that extraction for element in rice, dry ashing method is because to be consumed energy high by the way of high temperature sintering
And easily lead to the loss of tested element；The shortcomings that wet digestion is that time-consuming, can use a large amount of strong acid and strong oxidizer, and disappear
Toxic exhaust gas can be generated in solution preocess；Relative to traditional wet digestion, the time-consuming of Microwave Digestion is shorter, but cools down at last
The time of decompression, primary resolution usually time-consuming 1 more than hour；The amount of strong acid and strong oxidizer that Microwave Digestion needs is opposite
It is less, but need to use microwave dissolver costly to realize the closed environment of high temperature and pressure.
Extraction of the ultrasonic wave added enzymatic isolation method being reported in recent years for element in rice, does not need using strong acid and strong oxygen
Agent, time-consuming are significantly less than micro-wave digestion.But primary enzymolysis, which can only quantify, extracts a kind of element in rice, and time of other elements
Yield cannot ensure, significantly limit the practical application of such method.
Summary of the invention
The purpose of the present invention is to provide a kind of sides by trace arsenic in rice kernels, four kinds of cadmium, manganese and zinc element extractions into solution
Method, this method can simultaneously rapidly extracting trace arsenic in rice kernels, cadmium, manganese and zinc.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of methods by trace arsenic in rice kernels, four kinds of cadmium, manganese and zinc element extractions into solution, including with
Lower step:
1) rice meal and pancreas enzyme -EDTA extract liquor are mixed, carries out ultrasound, obtains ultrasonic enzymolysis liquid；
2) ultrasound enzymolysis liquid described in step 1) is centrifuged, obtains the first supernatant and substrate, takes substrate and nitric acid aqueous solution
Solution mixing, centrifugation obtain the second supernatant；
3) first supernatant is merged with the second supernatant, obtains the extracting solution of trace arsenic in rice kernels, cadmium, manganese and zinc；
Pancreas enzyme -EDTA extract liquor described in step 1) includes pancreatin, ethylenediamine tetra-acetic acid and phosphate buffer solution；It is described
The concentration of pancreatin is 1.5~3.5g/L in pancreas enzyme -EDTA extract liquor；Ethylenediamine tetra-acetic acid in the pancreas enzyme -EDTA extract liquor
Concentration is 0.1~0.3g/L；The total concentration of phosphate radical is 0.005~0.015mol/L in the pancreas enzyme -EDTA extract liquor.
Preferably, the pH value of pancreas enzyme -EDTA extract liquor described in step 1) is 7.5~8.6.
Preferably, the mixed proportion of rice meal described in step 1) and pancreas enzyme -EDTA extract liquor be 10~40mg:800~
1000μL。
Preferably, temperature ultrasonic described in step 1) is 15~37 DEG C；The time of the ultrasound is 2~25 minutes；Institute
The frequency for stating ultrasound is 20~80kHz；The power of the ultrasound is 400~800W.
Preferably, partial size≤75 μm of rice meal described in step 1).
Preferably, the volumn concentration of nitric acid is 1%~3% in aqueous solution of nitric acid described in step 2).
Preferably, the revolving speed of centrifugation described in step 2) is 3000~5000rpm；The time of the centrifugation is 5~10 points
Clock.
It preferably, will using aqueous solution of nitric acid after the extracting solution that step 3) obtains the trace arsenic in rice kernels, cadmium, manganese and zinc
Extracting solution constant volume is to 4~10mL, through membrane filtration, detects wherein each element content with elemental analysis instrument.
Beneficial effects of the present invention: the present invention provides a kind of by four kinds of trace arsenic in rice kernels, cadmium, manganese and zinc element extractions to molten
Method in liquid.The present invention joined complexing agent ethylenediamine tetra-acetic acid while digesting using pancreatin to rice meal
(Ethylenediaminetetraacetic acid, EDTA), improves the rate of recovery of heavy metal element.In addition, the present invention couple
Substrate after enzymatic hydrolysis carries out a pickling, to further improve the rate of recovery of element.Method of the invention can be at 20 points
(timing since the rice crushed, to the filtering for completing extracting solution) is by four kinds of trace arsenic in rice kernels, cadmium, manganese, zinc members in clock
Element is quantitative to be extracted in solution, compared to traditional elemental analysis pretreatment technology, is significantly shortened the processing time, is avoided
The use of strong oxidizer reduces strong acid usage amount and energy consumption, compares other zymolysis techniques, realizes multielement in rice for the first time
While quantitatively extract.
Specific embodiment
The present invention provides a kind of methods by trace arsenic in rice kernels, four kinds of cadmium, manganese and zinc element extractions into solution, including with
Lower step:
1) rice meal and pancreas enzyme -EDTA extract liquor are mixed, carries out ultrasound, obtains ultrasonic enzymolysis liquid；
2) ultrasound enzymolysis liquid described in step 1) is centrifuged, obtains the first supernatant and substrate, takes substrate and nitric acid aqueous solution
Solution mixing, centrifugation obtain the second supernatant；
3) first supernatant is merged with the second supernatant, obtains the extracting solution of trace arsenic in rice kernels, cadmium, manganese and zinc；
Pancreas enzyme -EDTA extract liquor described in step 1) includes pancreatin, ethylenediamine tetra-acetic acid and phosphate buffer solution；It is described
The concentration of pancreatin is 1.5~3.5g/L in pancreas enzyme -EDTA extract liquor；Ethylenediamine tetra-acetic acid in the pancreas enzyme -EDTA extract liquor
Concentration is 0.1~0.3g/L；The total concentration of phosphate radical is 0.005~0.015mol/L in the pancreas enzyme -EDTA extract liquor.
The present invention crushes rice to obtain rice meal, rice meal and the mixing of pancreas enzyme -EDTA extract liquor first, carries out ultrasound,
Obtain ultrasonic enzymolysis liquid；The partial size of the rice meal is preferred≤and 75 μm；The concentration of pancreatin is excellent in the pancreas enzyme -EDTA extract liquor
It is selected as 2~3g/L, more preferably 2.5g/L；The concentration of ethylenediamine tetra-acetic acid is preferably 0.2g/ in the pancreas enzyme -EDTA extract liquor
L；The total concentration of phosphate radical is preferably 0.01mol/L in the pancreas enzyme -EDTA extract liquor；The pH of the pancreas enzyme -EDTA extract liquor
Value preferably 7.5~8.6, more preferably 8；The dosage of the rice meal is preferably 10~50mg, more preferably 20~40mg, most
Preferably 30mg；The mixed proportion of the rice meal and pancreas enzyme -EDTA extract liquor is preferably the μ L of 10~40mg:800~1000, more
Preferably 30mg:900 μ L；The temperature of the ultrasound is preferably 15~37 DEG C, more preferably 20~30 DEG C, most preferably 25 DEG C；
The time of the ultrasound is preferably 2~25 minutes, more preferably 5~20 minutes, most preferably 5 minutes；The frequency of the ultrasound
Preferably 20~80kHz, more preferably 40~60kHz, most preferably 50kHz；The power of the ultrasound is preferably 400~
800W, more preferably 500~700W, most preferably 600W.
In the present invention, the EDTA has the advantages that complexing power is strong and is not easy to be biodegradable.
After obtaining ultrasonic enzymolysis liquid, the present invention is centrifuged the ultrasonic enzymolysis liquid, obtains the first supernatant and substrate,
Substrate is taken to mix with aqueous solution of nitric acid, centrifugation obtains the second supernatant；The revolving speed of the centrifugation is preferably 3000~5000rpm,
More preferably 4000rpm；The time of the centrifugation is preferably 5~10 minutes, and more preferably 6~8 minutes；The temperature of the centrifugation
Preferably 20~35 DEG C, more preferably 25~30 DEG C；In the aqueous solution of nitric acid volumn concentration of nitric acid be preferably 1%~
3%, more preferably 2%；The dosage of the aqueous solution of nitric acid is preferably 1.5mL.
The present invention merges first supernatant with the second supernatant to arrive the extraction of trace arsenic in rice kernels, cadmium, manganese and zinc
Liquid；It preferably further include using aqueous solution of nitric acid by extracting solution after the extracting solution for obtaining the trace arsenic in rice kernels, cadmium, manganese and zinc
Constant volume is to 4~10mL, through membrane filtration, detects wherein each element content with elemental analysis instrument.
In the present invention, the volumn concentration of nitric acid is preferably 1%~3% in the aqueous solution of nitric acid, more preferably
2%；The aperture of the filter membrane is preferably 0.45 μm.The elemental analysis instrument includes inductivity coupled plasma mass spectrometry, inductance
Coupled plasma spectroscopy or graphite furnace atomic absorption spectrometry etc..
Technical solution provided by the invention is described in detail below with reference to embodiment, but they cannot be understood
For limiting the scope of the present invention.
A kind of method by trace arsenic in rice kernels, four kinds of cadmium, manganese and zinc element extractions into solution of embodiment 1
Rice material: GBW (E) 100348, GBW10043 and GBW10044；
Method:
1. configuring pancreas enzyme -EDTA extract liquor, wherein pancreas enzyme concentration is 2.5g/L, ethylenediamine tetra-acetic acid
(Ethylenediaminetetraacetic acid, EDTA) concentration is 0.2g/L, phosphate buffer solution, wherein phosphate radical
Total concentration is 0.01mol/L, pH 8.0；
2. weighing 30mg GBW (E) 100348, GBW10043 and GBW10044 respectively, being uniformly crushed to partial size is 50~70
900 μ L pancreas enzyme -EDTA extract liquors are added after μm, under the conditions of 37 DEG C, ultrasound obtains for 5 minutes, supersonic frequency 60kHz, power 600W
To ultrasonic enzymolysis liquid；
3. ultrasonic enzymolysis liquid is centrifuged after five minutes under the conditions of 25 DEG C with the revolving speed of 4000rpm, supernatant is decanted off standby
With, the aqueous solution of nitric acid that 1.5mL volume fraction is 2% is added in substrate, it is uniformly mixed；
4. the mixture after aqueous solution of nitric acid will be added to be centrifuged 6 minutes with the revolving speed of 4000rpm at normal temperature, will be centrifuged twice
Obtained supernatant merges, and the aqueous solution of nitric acid constant volume for being 2% with volume fraction is to 5mL, after 0.45 μm of membrane filtration, power transmission
Sense coupled plasma mass spectrometry is detected.Extraction time is no more than 20 minutes, and testing result is referring to table 1.It uses as shown in Table 1
This method extract three kinds of Standard for Rice substances in arsenic, cadmium, four kinds of manganese, zinc elements, the rate of recovery in 80%~108% range,
Precision reaches the requirement of quantitative analysis in 4.1%~8.2% range.
The testing result of 1 Standard for Rice substance of table
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (8)
1. a kind of method by trace arsenic in rice kernels, four kinds of cadmium, manganese and zinc element extractions into solution, comprising the following steps:
1) rice meal and pancreas enzyme -EDTA extract liquor are mixed, carries out ultrasound, obtains ultrasonic enzymolysis liquid；
2) ultrasound enzymolysis liquid described in step 1) is centrifuged, obtains the first supernatant and substrate, takes substrate and aqueous solution of nitric acid
Mixing, centrifugation obtain the second supernatant；
3) first supernatant is merged with the second supernatant, obtains the extracting solution of trace arsenic in rice kernels, cadmium, manganese and zinc；
Pancreas enzyme -EDTA extract liquor described in step 1) includes pancreatin, ethylenediamine tetra-acetic acid and phosphate buffer solution；The pancreas
The concentration of pancreatin is 1.5~3.5g/L in enzyme-EDTA extract liquor；Ethylenediamine tetra-acetic acid is dense in the pancreas enzyme -EDTA extract liquor
Degree is 0.1~0.3g/L；The total concentration of phosphate radical is 0.005~0.015mol/L in the pancreas enzyme -EDTA extract liquor.
2. the method according to claim 1, wherein the pH value of pancreas enzyme -EDTA extract liquor described in step 1) is
7.5~8.6.
3. method according to claim 1 or 2, which is characterized in that rice meal described in step 1) and pancreas enzyme -EDTA extraction
The mixed proportion of liquid is the μ of 10~40mg:800~1000 L.
4. according to the method described in claim 3, it is characterized in that, temperature ultrasonic described in step 1) is 15~37 DEG C；Institute
The time for stating ultrasound is 2~25 minutes；The frequency of the ultrasound is 20~80kHz；The power of the ultrasound is 400~800 W.
5. the method according to claim 1, wherein partial size≤75 μm of rice meal described in step 1).
6. the method according to claim 1, wherein in aqueous solution of nitric acid described in step 2) nitric acid volume hundred
Dividing content is 1%~3%.
7. the method according to claim 1, wherein the revolving speed of centrifugation described in step 2) be 3000~
5000rpm；The time of the centrifugation is 5~10 minutes.
8. the method according to claim 1, wherein obtaining the trace arsenic in rice kernels, cadmium, manganese and zinc in step 3)
It further include using aqueous solution of nitric acid by extracting solution constant volume to 4~10mL, through membrane filtration, with elemental analysis instrument after extracting solution
Detect wherein each element content.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106198412A (en) * | 2015-05-04 | 2016-12-07 | 内蒙古蒙牛乳业（集团）股份有限公司 | The detection method of constituent content in a kind of food |
| CN107167353A (en) * | 2017-07-05 | 2017-09-15 | 赛思莱（厦门）生物科技有限公司 | A kind of sample preparation processing method for the grand protein science research of soil |
-
2019
- 2019-07-26 CN CN201910681423.7A patent/CN110361249A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106198412A (en) * | 2015-05-04 | 2016-12-07 | 内蒙古蒙牛乳业（集团）股份有限公司 | The detection method of constituent content in a kind of food |
| CN107167353A (en) * | 2017-07-05 | 2017-09-15 | 赛思莱（厦门）生物科技有限公司 | A kind of sample preparation processing method for the grand protein science research of soil |
Non-Patent Citations (3)
| Title |
|---|
| 程宝鸾主编: "《动物细胞培养技术》", 31 March 2000, 程宝鸾主编 * |
| 臧广州 主编: "《药品检验监测技术操作规划与药品质量监管执法制度实务全书》", 28 February 2005, 银声音像出版社 * |
| 赵尔敏 等: "ICP-MS直接进样对大米酶解液中痕量硒的测定", 《食品科学》 * |
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