CN106918589A - A kind of method of potassium ion in quick measure fruit - Google Patents
A kind of method of potassium ion in quick measure fruit Download PDFInfo
- Publication number
- CN106918589A CN106918589A CN201710291854.3A CN201710291854A CN106918589A CN 106918589 A CN106918589 A CN 106918589A CN 201710291854 A CN201710291854 A CN 201710291854A CN 106918589 A CN106918589 A CN 106918589A
- Authority
- CN
- China
- Prior art keywords
- potassium
- solution
- sample
- standard
- volumetric flasks
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
Landscapes
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Plasma & Fusion (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention belongs to technical field of food detection, and in particular to the method for potassium ion, the method in a kind of quick measure fruit through the following steps that realize：Ultrasonic extraction：Sample is weighed in centrifuge tube, is added water, after ultrasonic extraction cooling, add cesium chloride solution, nitric acid, constant volume, filtering；Solid-phase extraction column is crossed, is collected and is all crossed post solution and constant volume；The drafting of standard curve；Sample determination：The solution after post was taken, was determined using inductive coupling plasma emission spectrograph, it is quantitative according to standard curve.The present invention avoids carrying out the Specimen eliminating of complexity using the extract solution that potassium in simple extraction acquisition fruit is determined, and method is simple and easy to apply, can largely save the time of sample pre-treatments, improves detection efficiency.
Description
Technical field
The invention belongs to technical field of food detection, and in particular to a kind of method of potassium ion in quick measure fruit.
Background technology
Potassium has the important function for maintaining human normal physiological function, participates in energetic supersession and maintenance is nervimuscular just
Chang Gongneng.When internal potassium deficiency, general weakness, tired, heartbeat can be caused to weaken, feel dizzy, severe potassium deficiency is also resulted in exhales
Inhale myoparalysis dead.Additionally, low potassium can slow down gastrointestinal peristalsis, cause enteroparalysis, aggravate apocleisis, Nausea and vomiting, abdominal distension occur
Etc. symptom.Human body is photographed the exclusion that appropriate potassium is beneficial to internal unnecessary sodium, especially significant to hyperpietic.
At present, the sides such as the pre-treating method that potassium content is determined in fruit mainly has dry method to clear up, Wet, micro-wave digestion
Method.Dry method is cleared up needs the steps such as charing, high temperature ashing, dissolving with hydrochloric acid, clears up the cycle for 4-6 hour, potassium in digestion process
Easily loss, the rate of recovery is low；Wet needs to add the oxidants such as a large amount of nitric acid, hydrogen peroxide, perchloric acid to clear up, and clears up the cycle
It it is 3-5 hours, because the reagent for needing is more, blank value is higher, the control of digestion process conditional is bad easy to explode；Microwave disappears
Solution needs the special microwave dissolver of purchase, clears up reagent for nitric acid and hydrogen peroxide, clears up the cycle for 3-4 hours.Place before these
The shortcoming of reason is to need more complicated instrument, and pre-treating method is cumbersome, time-consuming, laborious, and blank value is higher.
The content of the invention
For problems of the prior art, the invention provides a kind of method of potassium ion in quick measure fruit.
Concrete technical scheme of the present invention is as follows：
The invention provides a kind of method of potassium ion in quick measure fruit, comprise the following steps：
（1）Ultrasonic extraction：Sample that 2.00g crushes is weighed in 50mL centrifuge tubes, add water 30mL, turns after ultrasonic extraction cooling
50mL volumetric flasks are moved to, 10% cesium chloride solution 1mL, nitric acid 1mL is added, scale is settled to, filter paper filters to take filtrate；
（2）Cross solid-phase extraction column：The solid phase extraction column of activation is selected, 5mL filtrates is accurately pipetted and is crossed post, heated in advance with 5mL
To 60 DEG C of milli-Q water 3 times, collected with 25mL volumetric flasks and all cross post solution and constant volume；
（3）The drafting of standard curve：Configuration potassium ion standard liquid, takes 100mL volumetric flasks, is settled to scale, takes ultra-pure water and adds
Enter 10% cesium chloride solution 2mL, nitric acid 2mL, be settled to scale, as standard blank, inductively coupled plasma is then used successively
Body emission spectrometer is determined, and draws standard curve；
（4）Sample determination：The solution after post was taken, was determined using inductive coupling plasma emission spectrograph, it is bent according to standard
Line is quantified.
Further, the condition of the ultrasound is the ultrasonic extraction 30min at 60 DEG C.
Solid phase extraction column used in the present invention is Oasis®HLB。
Above-mentioned solid phase extraction pillar activation method be：Solid phase extraction column is heated in advance with 6mL methyl alcohol and 6mL successively
Activated to 60 DEG C of ultra-pure waters.
Further, the collocation method of the potassium ion standard liquid is：Take the potassium standard that 10mL concentration is 1000mg/L
Solution, using pure water solution constant volume, obtains the potassium standard liquid of 100mg/L in 100mL volumetric flasks, takes the potassium mark of 100mg/L
Quasi- solution 1mL, 2mL, 3mL, 4mL, 5mL add 10% cesium chloride solution 2mL, nitric acid 2mL in 100mL volumetric flasks, are settled to quarter
Degree, obtains the potassium standard liquid of 1mg/L, 2mg/L, 3mg/L, 4mg/L, 5mg/L.
Further, the inductive coupling plasma emission spectrograph condition determination is：
Determine wavelength：766.430nm,
Plasma flow：10L/min,
Secondary air amount：0.2L/min,
Nebulizer flow：0.55L/min,
Sample introduction speed：1.00mL/min,
Observed direction：Axially,
Observed range：15.
10% cesium chloride solution used in the present invention refers to mass concentration.
Beneficial effects of the present invention are：
（1）The present invention avoids carrying out the Specimen eliminating of complexity, method using the extract solution that potassium in simple extraction acquisition fruit is determined
It is simple and easy to apply, the time of sample pre-treatments can be largely saved, improve detection efficiency；
（2）Currently preferred solid phase extraction column can be surveyed effectively the small organic molecule such as place to go pectic substance, organic acid to potassium
Surely the Matrix effects for causing, improve the degree of accuracy of potassium measure.
（3）The present invention avoids carrying out Specimen eliminating using a large amount of acid, so as to reduce sample blank caused by acid adding.
（4）Compared with traditional Specimen eliminating pre-treating method, this method time for sample pretreatment can shorten 30%-
80%, the detection efficiency of potassium measure in fruit can be improved.
Brief description of the drawings
Fig. 1 is the potassium standard curve that embodiment 1 is determined.
Fig. 2 is the potassium standard curve that comparative example 1 is determined.
Specific embodiment
Instantiation mode with reference to embodiments is described in further detail to the above of the invention again, but
This scope for being interpreted as above-mentioned theme of the invention should not be only limitted to following embodiment.
Embodiment 1
The method of potassium ion, comprises the following steps in a kind of quick measure apple：
（1）Ultrasonic extraction：Sample that the apple 2.00g of two types of in the market crushes is weighed in 50mL centrifuge tubes, is added
30mL water, ultrasonic extraction 30min at 60 DEG C is transferred to 50mL volumetric flasks after cooling, add 10% cesium chloride solution 1mL, top grade
Pure nitric acid 1mL, is settled to scale, and filter paper filters to take filtrate；
（2）Cross solid-phase extraction column：By Oasis®HLB solid phase extraction columns are previously heated to 60 DEG C with 6mL methyl alcohol and 6mL successively
Ultra-pure water is activated, and is accurately pipetted 5mL filtrates and is crossed post, and 60 DEG C of milli-Q water 3 times is previously heated to 5mL, uses 25mL capacity
Bottle is collected and all crosses post solution and constant volume；
（3）The drafting of standard curve：Potassium ion standard liquid is prepared, ultra-pure water is taken as standard blank, adds 10% cesium chloride molten
Then liquid 2mL, nitric acid 2mL, constant volume is determined using inductive coupling plasma emission spectrograph successively, draws standard curve；
The collocation method of the potassium ion standard liquid is：The potassium standard liquid that 10mL concentration is 1000mg/L is taken to hold in 100mL
In measuring bottle, using pure water solution constant volume, obtain the potassium standard liquid of 100mg/L, take the potassium standard liquid 1mL of 100mg/L, 2mL,
3mL, 4mL, 5mL add 10% cesium chloride solution 2mL, nitric acid 2mL in 100mL volumetric flasks, constant volume obtain 1mg/L, 2mg/L,
The potassium standard liquid of 3mg/L, 4mg/L, 5mg/L；As shown in Figure 1, this determination of experimental method result is linearly：R2=0.9993；
（4）Sample determination：The solution after post was taken, was determined using inductive coupling plasma emission spectrograph, it is bent according to standard
Line is quantified；
The inductive coupling plasma emission spectrograph condition determination is：
Determine wavelength：766.430nm,
Plasma flow：10L/min,
Secondary air amount：0.2L/min,
Nebulizer flow：0.55L/min,
Sample introduction speed：1.00mL/min,
Observed direction：Axially,
Observed range：15.
Each sample does three mark-ons of different levels, and sample and mark-on are determined 6 times averages as end value.Determine
The results are shown in Table 1, table 2.
Table 1
Table 2
Comparative example 1
Pre-treatment is carried out using most micro-wave digestions using current domestic laboratory, when preparing graticule 2% nitric acid need to be added to enter
Row acid Matrix Match, specific experiment operating process is as follows：
（1）Sample microwave treatment：Sample 2.00g is weighed in polytetrafluoroethylene (PTFE) counteracting tank, 8mL nitric acid and 2mL hydrogen peroxide is added,
Cleared up in microwave dissolver, micro-wave digestion condition is：120 DEG C of holdings 10min, 160 DEG C of holding 20min, 190 keep
20min；Power is 1200W.Ultrapure water counteracting tank lid and inwall to polytetrafluoroethylene (PTFE) are used after clearing up completion cooling 30min
In counteracting tank, then in catching up with sour electric hot plate to catch up with sour 100min, testing sample solution is obtained；
（2）Preparing standard solution：Take 10mL concentration be 1000mg/L potassium standard liquid in 100mL volumetric flasks, use volume integral
Number is 2% aqueous solution of nitric acid constant volume, obtains the potassium standard liquid of 100mg/L, take the potassium standard liquid 2mL of 100mg/L, 4mL,
6mL, 8mL, 10mL in the aqueous solution of nitric acid constant volume that 100mL volumetric flask volume fractions are 2% obtain 2mg/L, 4mg/L, 6mg/L,
The potassium standard liquid of 8mg/L, 10mg/L；
Draw standard curve：Take the aqueous solution of nitric acid that volume fraction is 2% molten as standard liquid blank, and the standard of preparation
Liquid dilution, standard curve is drawn out according to response；From figure 2 it can be seen that potassium standard curve is linearly R2=
0.99921；
（3）Sample determination：Step 1）Testing sample solution is transferred in 50mL volumetric flasks, and poly- four are repeatedly rinsed with a small amount of ultra-pure water
The counteracting tank of PVF is simultaneously transferred in 50mL volumetric flasks, after then being mixed with ultra-pure water constant volume, uses inductively coupled plasma
Body emission spectrometer is determined.
Inductive coupling plasma emission spectrograph condition determination is the same, and specific measurement result is shown in Table 3 and table 4.
Table 3
Table 4
The method that comparative example 1 is provided is the determination method that major part laboratory uses at present, the time of pre-treatment and the inventive method
Compare：Need proprietary microwave dissolver, the time lengthening of pre-treatment 2-3 hour, and complex operation step, to testing skill
Energy requirement is higher, increased the uncertain of experimental result.This fully demonstrates practicality of the invention.
Comparative example 2
The method of potassium ion, comprises the following steps in a kind of quick measure apple：
（1）Ultrasonic extraction：Sample that the apple 2.00g of two types of in the market crushes is weighed in 50mL centrifuge tubes, is added
30mL water, ultrasonic extraction 30min at 60 DEG C is transferred to 50mL volumetric flasks after cooling, top pure grade nitric acid 1mL is settled to scale,
Filter paper filters to take filtrate；
（2）Cross solid-phase extraction column：By Oasis®HLB solid phase extraction columns are previously heated to 60 DEG C with 6mL methyl alcohol and 6mL successively
Ultra-pure water is activated, and is accurately pipetted 5mL filtrates and is crossed post, and 60 DEG C of milli-Q water 3 times is previously heated to 5mL, uses 25mL capacity
Bottle is collected and all crosses post solution and constant volume；
（3）The drafting of standard curve：Method is with embodiment 1；
（4）Sample determination：The solution after post was taken, was determined using inductive coupling plasma emission spectrograph（Testing conditions are same
Embodiment 1）, it is quantitative according to standard curve；
Each sample does three mark-ons of different levels, and sample and mark-on are determined 6 times averages as end value.Measurement result
It is shown in Table 5, table 6.
Table 5
Table 6
Comparative example 3
The method of potassium ion, comprises the following steps in a kind of quick measure apple：
（1）Ultrasonic extraction：Sample that the apple 2.00g of two types of in the market crushes is weighed in 50mL centrifuge tubes, is added
30mL water, ultrasonic extraction 30min at 60 DEG C, is transferred to 50mL volumetric flasks after cooling, be settled to scale, and filter paper filters to take filtrate；
（2）The drafting of standard curve：Method is with embodiment 1；
（3）Sample determination：Solution to be measured is taken, is determined using inductive coupling plasma emission spectrograph（Testing conditions are with implementation
Example 1）, it is quantitative according to standard curve；
Each sample does three mark-ons of different levels, and sample and mark-on are determined 6 times averages as end value.Measurement result
It is shown in Table 7, table 8.
Table 7
Table 8
Claims (6)
1. in a kind of quick measure fruit potassium ion method, it is characterised in that comprise the following steps：
（1）Ultrasonic extraction：Sample that 2.00g crushes is weighed in 50mL centrifuge tubes, add water 30mL, turns after ultrasonic extraction cooling
50mL volumetric flasks are moved to, 10% cesium chloride solution 1mL, nitric acid 1mL is added, scale is settled to, filter paper filters to take filtrate；
（2）Cross solid-phase extraction column：The solid phase extraction column of activation is selected, 5mL filtrates is accurately pipetted and is crossed post, heated in advance with 5mL
To 60 DEG C of milli-Q water 3 times, collected with 25mL volumetric flasks and all cross post solution and constant volume；
（3）The drafting of standard curve：Configuration potassium ion standard liquid；100mL volumetric flasks are taken, 10% cesium chloride solution 2mL is added,
Nitric acid 2mL, is settled to scale, as standard blank, is then determined using inductive coupling plasma emission spectrograph successively, paints
Standard curve processed；
（4）Sample determination：The solution after post was taken, was determined using inductive coupling plasma emission spectrograph, it is bent according to standard
Line is quantified.
2. method according to claim 1, it is characterised in that the condition of the ultrasound is the ultrasonic extraction at 60 DEG C
30min。
3. method according to claim 1, it is characterised in that the solid phase extraction column is Oasis®HLB。
4. method according to claim 3, it is characterised in that the method for the activation is：By solid phase extraction column successively
The ultra-pure water for being previously heated to 60 DEG C with 6mL methyl alcohol and 6mL is activated.
5. method according to claim 1, it is characterised in that the collocation method of the potassium ion standard liquid is：Take
10mL concentration for 1000mg/L potassium standard liquid in 100mL volumetric flasks, using pure water solution constant volume, obtain 100mg/L's
Potassium standard liquid, takes potassium standard liquid 1mL, 2mL, 3mL, 4mL, 5mL of 100mg/L in 100mL volumetric flasks, adds 10% chlorination
Caesium solution 2mL, nitric acid 2mL, are settled to scale, obtain the potassium standard liquid of 1mg/L, 2mg/L, 3mg/L, 4mg/L, 5mg/L.
6. the method according to claim any one of 1-5, it is characterised in that the inductively coupled plasma atomic emission
Instrument condition determination is：
Determine wavelength：766.430nm,
Plasma flow：10L/min,
Secondary air amount：0.2L/min,
Nebulizer flow：0.55L/min,
Sample introduction speed：1.00mL/min,
Observed direction：Axially,
Observed range：15.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710291854.3A CN106918589A (en) | 2017-04-28 | 2017-04-28 | A kind of method of potassium ion in quick measure fruit |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710291854.3A CN106918589A (en) | 2017-04-28 | 2017-04-28 | A kind of method of potassium ion in quick measure fruit |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106918589A true CN106918589A (en) | 2017-07-04 |
Family
ID=59567739
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710291854.3A Pending CN106918589A (en) | 2017-04-28 | 2017-04-28 | A kind of method of potassium ion in quick measure fruit |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106918589A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110487619A (en) * | 2019-07-31 | 2019-11-22 | 河钢股份有限公司承德分公司 | A method of potassium content in measurement vanadium slag sintering additives |
-
2017
- 2017-04-28 CN CN201710291854.3A patent/CN106918589A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110487619A (en) * | 2019-07-31 | 2019-11-22 | 河钢股份有限公司承德分公司 | A method of potassium content in measurement vanadium slag sintering additives |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Yilmaz et al. | Ionic liquid-linked dual magnetic microextraction of lead (II) from environmental samples prior to its micro-sampling flame atomic absorption spectrometric determination | |
| Yilmaz et al. | Switchable solvent-based liquid phase microextraction of copper (II): optimization and application to environmental samples | |
| CN106093289B (en) | The continuous extraction method of different organic components in soil | |
| Guo et al. | Trace determination of selenium in biological samples by CH4-Ar mixed gas plasma DRC-ICP-MS | |
| CN104697983A (en) | Method of detecting heavy metal lead, cadmium, arsenic and copper in TCM (Traditional Chinese Medicine) tablet | |
| Sun et al. | Simultaneous determination of trace arsenic (III), antimony (III), total arsenic and antimony in Chinese medicinal herbs by hydride generation-double channel atomic fluorescence spectrometry | |
| CN103543055A (en) | Pretreatment method for heavy metal element detection in solid sample and application of pretreatment method | |
| Li et al. | Cloud point extraction for trace inorganic arsenic speciation analysis in water samples by hydride generation atomic fluorescence spectrometry | |
| Duarte et al. | Seafood digestion by microwave-induced combustion for total arsenic determination by atomic spectrometry techniques with hydride generation | |
| Gao et al. | On-line UV photochemical generation of volatile copper species and its analytical application | |
| CN103604686B (en) | The pre-treatment of rapid determination of content of cadmium element and quantitative analysis method in a kind of Fast Measurement rice | |
| CN103822999A (en) | Full-automatic QuEChERS preprocessing all-in-one machine and preprocessing method | |
| Shirkhanloo et al. | Ultra-trace arsenic and mercury speciation and determination in blood samples by ionic liquid-based dispersive liquid-liquid microextraction combined with flow injection-hydride generation/cold vapor atomic absorption spectroscopy | |
| CN110779901B (en) | Ratiometric probe based on internal filtering effect and construction method and application thereof | |
| Zeng et al. | Chemical vapor generation of bismuth in non-aqueous phase based on cloud point extraction coupled with thermospray flame furnace atomic absorption spectrometric determination | |
| Yang et al. | Micro-spectrophotometric determination of nickel in Gentiana rigescens after switchable hydrophilicity solvent-based ultrasound-assisted liquid phase microextraction | |
| CN101813630B (en) | Method for detecting molybdenum element in milk powder | |
| CN106908530A (en) | IC ICP MS combinations determine method and the application of Arsenic in tea form | |
| He et al. | Simultaneous determination of Cd and Ni in Salvia yunnanensis by deep eutectic solvent-based rapidly synergistic cloud point extraction and ICP-OES analysis | |
| Li et al. | UV photochemical vapor generation–nitrogen microwave induced plasma optical emission spectrometric determination of nickel | |
| CN106918589A (en) | A kind of method of potassium ion in quick measure fruit | |
| Huang et al. | Infrared-assisted extraction coupled with high performance liquid chromatography (HPLC) for determination of liquiritin and glycyrrhizic acid in licorice root | |
| CN107748153A (en) | A kind of penicillamine probe of fluorescent ultraviolet dual signal model and its application | |
| Liu et al. | A novel gas liquid separator for direct sampling analysis of ultratrace arsenic in blood sample by hydride generation in-situ dielectric barrier discharge atomic fluorescence spectrometry | |
| CN109212108A (en) | Gas chromatography-mass spectrometry that is a kind of while measuring three kinds of trace quinolines herbicides in rice and soybean |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170704 |
|
| WD01 | Invention patent application deemed withdrawn after publication |