CN110320207A - A kind of iodine detection reagent and detection method - Google Patents
A kind of iodine detection reagent and detection method Download PDFInfo
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- CN110320207A CN110320207A CN201910664099.8A CN201910664099A CN110320207A CN 110320207 A CN110320207 A CN 110320207A CN 201910664099 A CN201910664099 A CN 201910664099A CN 110320207 A CN110320207 A CN 110320207A
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Abstract
The present invention relates to a kind of iodine detection reagents, including digestion solution, neutralizer, indicator, the Oxidizing and Reducing Agents being retained separately, the oxidant is the sulfuric acid solution of quadrivalent cerium, and the concentration of the quadrivalent cerium is 0.04~15mol/L, and the concentration of the sulfuric acid is 0.05~9mol/L.Iodine detection reagent of the invention increases stability of the oxidant in metachromasia, so that reaction power regression curve time and detected value goodness of fit coefficient R value can achieve 0.9995 or more, simultaneously, so that the margi n pulls big between the iodide ion metachromasia time of various concentration, the detection sensitivity and accuracy of the iodide ion of high concentration are increased, so that an iodide ion detection range can achieve 1-2000 μ g/L.
Description
Technical field
The present invention relates to iodine detection technique fields, and in particular to a kind of iodine detection reagent and detection method.
Background technique
Iodine be in the life of the mankind it is extremely important, human body each period is required to.It can adjust energetic supersession, make
Energy-producing materials such as carbohydrate etc. generates energy, and supply cell utilizes, to complete various physiological activities;Importantly, iodine
The thyroid gland of generation can promote the intelligence and growth and development of infant, promote the proliferation and myelinization of cerebral neuron, especially
It is the foundation of dendron, dendritic spines and central nervous system.Meanwhile the thyroxine of iodine synthesis can promote the life in tricarboxylic acid cycle
Object oxidation adjusts energy conversion, the synthesis of regulatory protein matter and decomposition, promotes sugar and fat metabolism, accelerate being absorbed and utilized for sugar, promote
Sugar entering original and lipolysis oxidation, adjust serum cholesterol and phospholipid concentration etc..Country is for the shortage of iodine in human body and more
The disease that iodine is formed is paid much attention to, but all iodine detection is not included in detection range in many large hospitals so far, this master
If the epidemic situation comparison due to iodine is special, nature is mostly with the presence of compound iodide ion.
It is arsenic cerium redox spectrophotometer method that iodine detection method is recommended by country at present, which exists
It is complicated in operation, and handled before must being done before inspection for complex sample, while hot digestion must also be done in the detection process
Processing, reagent and sample because heating will appear volatility, indoor air environment is influenced it is big, while original method in the detection because
Human factor is big for the error of result, and detection time is long, poor accuracy, is unfavorable for operating using equipment automatization, in hospital
In can not all promote implementation till now, this be also why existing hospital it is few detection urine iodines project reasons.Its
His detection reagent method all is difficult to carry out because of inaccurate and too complicated in hospital so far.
A kind of fast quantitative urine iodine detecting reagent kit and detection method are provided in the patent of Patent No. CN1348097A,
Kit includes digestion solution, parsing agent, neutralizer, 6 group reagent of reducing agent, indicator and oxidant, interpretation result in use
When, not exclusively due to the reaction of various concentration iodine solution, color transient change, reaction time deviation is very big, while various concentration is anti-
Can not really be pulled open between seasonable, cause to measurement result can not accurate interpretation, cause large error, can not actually use, together
When reagent stability and validity it is all poor, temperature effect is sensitive, relatively low in 10 DEG C or so detected values.
Summary of the invention
It is good that technical problem to be solved by the invention is to provide a kind of stability, the high urine iodine iodine inspection of detection accuracy
Test agent and detection method.
The technical scheme to solve the above technical problems is that
In a first aspect, wrapping the digestion solution being retained separately the present invention provides a kind of iodine detection reagent, neutralizer, going back
Former agent, indicator and oxidant, the oxidant are the aqueous sulfuric acid of quadrivalent cerium, the concentration of the quadrivalent cerium is 0.04~
15mol/L, the concentration of the sulfuric acid are 0.05~9mol/L.
Further, the digestion solution is the aqueous solution for the sodium hypochlorite that concentration is 0.07~0.6mol/L.
Further, the digestion solution is the aqueous solution of sodium hypochlorite and sodium hydroxide, the sodium hypochlorite and the hydrogen-oxygen
The concentration for changing sodium is respectively 0.07~0.6mol/L and 0.1~2.5mol/L.
Further, the quadrivalent cerium is one or both of Cericammoniumsulfate or cerous sulfate.
Further, the neutralizer be one of sulfuric acid solution, hydrochloric acid solution, perchloric acid solution or sodium chlorate solution or
Several, the pH value of the neutralizer is less than 3.
Further, the reducing agent is the sodium arsenite aqueous solution that concentration is 0.05~1mol/L.
Further, the reducing agent is the aqueous solution of sodium arsenite and sodium chloride, the sodium arsenite and sodium chloride it is dense
Degree is respectively 0.05~1mol/L and 0.01~2mol/L.
Further, the indicator is the aqueous sulfuric acid of Ferroin reagent, the concentration of Phen in the indicator
For 0.005~1.6mol/L, the concentration of ferrous ion is 0.003~1.5mol/L, and the concentration of sulfuric acid is 0.01~1.5mol/L.
Further, the ferrous ion is selected from one or both of ferrous sulfate, iron ammonium sulfate or frerrous chloride.
The beneficial effects of the present invention are: the sulfuric acid in oxidant, increases stability of the oxidant in metachromasia, makes
It must react the power regression curve time and detected value goodness of fit coefficient R value can achieve 0.9995 or more, meanwhile, so that different
Margi n pulls big between the iodide ion metachromasia time of concentration increases the detection sensitivity of the iodide ion of high concentration and accurate
Property, so that an iodide ion detection range can achieve 1~2000 μ g/L;Degree of purity difference causes in the raw material of urea reagent
Consistency is poor in every batch of detection, and urea reagent is eliminated in the present invention, increases the consistency of batch detection;Hydrogen in digestion solution
Sodium oxide molybdena, improves validity period and the stability of digestion solution, to increase the validity period of iodine detection reagent of the invention
And stability.
On the other hand, the present invention also provides a kind of sides that iodine detection is carried out using above-mentioned iodine detection reagent
Method, specifically: iodine standard serial solution and sample liquid are taken, measuring respectively in identical reaction temperature joined the iodine inspection
Reaction time needed for the iodine standard serial solution of test agent reaches target absorbance value, and joined the iodine detection
Reaction time needed for the sample liquid of reagent reaches target absorbance value, joined the iodine standard of the iodine detection reagent
The reaction time of serial solution establishes standard curve with corresponding iodine concentration, by the standard curve and joined the iodine
Iodine content in sample liquid is calculated in the reaction time of the sample liquid of detection reagent.
Method of the invention is simple, and detection stability is good, and accuracy is high.
Specific embodiment
Principles and features of the present invention are described below in conjunction with specific embodiment, example is served only for explaining this hair
It is bright, it is not intended to limit the scope of the present invention.
Embodiment 1 prepares iodine detection reagent
3 groups of iodine detection reagents, respectively iodine detection reagent 1-1, iodine detection are prepared in the present embodiment altogether
Reagent 1-2 and iodine detection reagent 1-3.
The wherein formula of iodine detection reagent 1-1 are as follows: digestion solution is the aqueous sodium hypochlorite solution that concentration is 0.6mol/L,
Neutralizer is the sulfuric acid solution of 3.8mol/L, and the concentration of Phen is 1.6mol/L in indicator, ferrous sulfate concentration is
1mol/L, sulfuric acid concentration 1.5mol/L, reducing agent are the sodium arsenite aqueous solution that concentration is 1mol/L, and oxidant is cerous sulfate
Sulfuric acid solution, cerous sulfate vitriolization aqueous solution is prepared to obtain, wherein the concentration of cerous sulfate be 15mol/L, sulfuric acid it is dense
Degree is 9mol/L.
The formula of iodine detection reagent 1-2 are as follows: digestion solution is the aqueous sodium hypochlorite solution that concentration is 0.1mol/L, is neutralized
Agent is the hydrochloric acid solution of 1.5mol/L, and the concentration of Phen is 0.01mol/L in indicator, ferrous sulfate concentration is 1mol/
L, sulfuric acid concentration is 0.15mol/L, and reducing agent is the sodium arsenite aqueous solution that concentration is 0.5mol/L, and oxidant is Cericammoniumsulfate
Sulfuric acid solution, wherein the concentration of Cericammoniumsulfate is 4mol/L, the concentration of sulfuric acid is 0.5mol/L.
The formula of iodine detection reagent 1-3 are as follows: digestion solution is the aqueous sodium hypochlorite solution that concentration is 0.07mol/L, in
It is the perchloric acid solution of 0.1mol/L with agent, the concentration of Phen is 0.005mol/L in indicator, ferrous sulfate concentration is
0.003mol/L, sulfuric acid concentration 0.01mol/L, reducing agent are the sodium arsenite aqueous solution that concentration is 0.05mol/L, oxidant
For the sulfuric acid solution of cerous sulfate, wherein the concentration of cerous sulfate is 0.04mol/L, the concentration of sulfuric acid is 0.05mol/L.
Embodiment 2 prepares iodine detection reagent
3 groups of iodine detection reagents, respectively iodine detection reagent 2-1, iodine detection are prepared in the present embodiment altogether
Reagent 2-2 and iodine detection reagent 2-3.
The wherein formula of iodine detection reagent 2-1 are as follows: digestion solution is that concentration is the water-soluble of sodium hypochlorite and sodium hydroxide
Liquid, wherein the concentration of sodium hypochlorite is 0.6mol/L, and the concentration of sodium hydroxide is 2.5mol/L, and neutralizer is the sulphur of 5.5mol/L
Acid solution, the concentration of Phen is 1.6mol/L in indicator, ferrous sulfate concentration is 1mol/L, sulfuric acid concentration is
1.5mol/L, reducing agent are the sodium arsenite aqueous solution that concentration is 1mol/L, and oxidant is the sulfuric acid solution of cerous sulfate, wherein sulphur
The concentration of sour cerium is 15mol/L, the concentration of sulfuric acid is 9mol/L.
The formula of iodine detection reagent 2-2 are as follows: digestion solution is the aqueous solution that concentration is sodium hypochlorite and sodium hydroxide,
The concentration of middle sodium hypochlorite is 0.1mol/L, and the concentration of sodium hydroxide is 1mol/L, and neutralizer is the hydrochloric acid solution of 1.5mol/L,
Reducing agent is the sodium arsenite aqueous solution that concentration is 0.5mol/L, and the concentration of Phen is 0.01mol/L, sulfuric acid in indicator
Ferrous iron concentration is 1mol/L, sulfuric acid concentration 0.15mol/L, and oxidant is the sulfuric acid solution of Cericammoniumsulfate, wherein Cericammoniumsulfate
Concentration be 4mol/L, the concentration of sulfuric acid is 0.5mol/L.
The formula of iodine detection reagent 2-3 are as follows: digestion solution is the aqueous solution that concentration is sodium hypochlorite and sodium hydroxide,
The concentration of middle sodium hypochlorite is 0.07mol/L, and the concentration of sodium hydroxide is 0.1mol/L, and neutralizer is the perchloric acid of 0.1mol/L
Solution, reducing agent are the sodium arsenite aqueous solution that concentration is 0.05mol/L, and the concentration of Phen is in indicator
0.005mol/L, ferrous sulfate concentration is 0.003mol/L, sulfuric acid concentration 0.01mol/L, and oxidant is the sulfuric acid of cerous sulfate
Solution, wherein the concentration of cerous sulfate is 0.04mol/L, the concentration of sulfuric acid is 0.05mol/L.
Embodiment 3 prepares iodine detection reagent
5 groups of iodine detection reagents, respectively iodine detection reagent 3-1, iodine detection are prepared in the present embodiment altogether
Reagent 3-2, iodine detection reagent 3-3, iodine detection reagent 3-4 and iodine detection reagent 3-5.
The wherein formula of iodine detection reagent 3-1 are as follows: digestion solution is that concentration is the water-soluble of sodium hypochlorite and sodium hydroxide
Liquid, wherein the concentration of sodium hypochlorite is 0.07mol/L, and the concentration of sodium hydroxide is 0.1mol/L, and neutralizer is the sulphur of 1mol/L
Acid solution, reducing agent are the aqueous solution of sodium arsenite and sodium chloride, and wherein the concentration of sodium arsenite is 0.05mol/L, sodium chloride
Concentration be 0.01mol/L, the concentration of Phen is 0.005mol/L in indicator, ferrous sulfate concentration is 0.003mol/
L, sulfuric acid concentration is 0.01mol/L, and oxidant is the sulfuric acid solution of cerous sulfate, and wherein the concentration of cerous sulfate is 0.07mol/L, sulphur
The concentration of acid is 0.2mol/L.
The formula of iodine detection reagent 3-2 are as follows: digestion solution is the aqueous solution that concentration is sodium hypochlorite and sodium hydroxide,
The concentration of middle sodium hypochlorite is 0.1mol/L, and the concentration of sodium hydroxide is 0.5mol/L, and neutralizer is that the hydrochloric acid of 2.8mol/L is molten
Liquid, reducing agent are the aqueous solution of sodium arsenite and sodium chloride, and wherein the concentration of sodium arsenite is 0.1mol/L, the concentration of sodium chloride
For 0.8mol/L, the concentration of Phen is 0.6mol/L in indicator, frerrous chloride concentration is 1.5mol/L, sulfuric acid concentration is
0.1mol/L, oxidant are the sulfuric acid solution of Cericammoniumsulfate, and wherein the concentration of Cericammoniumsulfate is the concentration of 0.04mol/L, sulfuric acid
For 0.05mol/L.
The formula of iodine detection reagent 3-3 are as follows: digestion solution is the aqueous solution that concentration is sodium hypochlorite and sodium hydroxide,
The concentration of middle sodium hypochlorite is 0.5mol/L, and the concentration of sodium hydroxide is 2.5mol/L, and neutralizer is the perchloric acid of 2.5mol/L
Solution, reducing agent are the aqueous solution of sodium arsenite and sodium chloride, and wherein the concentration of sodium arsenite is 1mol/L, the concentration of sodium chloride
For 0.5mol/L, the concentration of Phen is 1.05mol/L in indicator, ferrous sulfate concentration is 1.05mol/L, sulfuric acid concentration
For 0.5mol/L, oxidant is the sulfuric acid solution of cerous sulfate, and wherein the concentration of cerous sulfate is 0.6mol/L, the concentration of sulfuric acid is
0.3mol/L。
The formula of iodine detection reagent 3-4 are as follows: digestion solution is the aqueous solution that concentration is sodium hypochlorite and sodium hydroxide,
The concentration of middle sodium hypochlorite is 0.6mol/L, and the concentration of sodium hydroxide is 2mol/L, and neutralizer is the sulfuric acid solution of 4.5mol/L,
Reducing agent is the aqueous solution of sodium arsenite and sodium chloride, and wherein the concentration of sodium arsenite is 1mol/L, and the concentration of sodium chloride is
1.5mol/L, the concentration of Phen is 0.2mol/L in indicator, ferrous sulfate concentration is 0.5mol/L, sulfuric acid concentration is
0.8mol/L oxidant is the sulfuric acid solution of cerous sulfate, and wherein the concentration of cerous sulfate is 15mol/L, the concentration of sulfuric acid is 9mol/
L。
The formula of iodine detection reagent 3-5 are as follows: digestion solution is the aqueous solution that concentration is sodium hypochlorite and sodium hydroxide,
The concentration of middle sodium hypochlorite is 0.2mol/L, and the concentration of sodium hydroxide is 1mol/L, and neutralizer is the sulfuric acid solution of 3.4mol/L,
Reducing agent is the aqueous solution of sodium arsenite and sodium chloride, and wherein the concentration of sodium arsenite is 0.9mol/L, and the concentration of sodium chloride is
2mol/L, the concentration of Phen is 1.6mol/L in indicator, ferrous sulfate concentration is 0.6mol/L, sulfuric acid concentration is
1.5mol/L, oxidant are the sulfuric acid solution of cerous sulfate, and wherein the concentration of cerous sulfate is 0.2mol/L, the concentration of sulfuric acid is
0.2mol/L。
Comparative example 1
Control iodine detection reagent is prepared in the method in the embodiment of the patent of Publication No. CN1348097A.
The detection method of 1 iodine of test example
Iodine standard serial solution and sample liquid are taken, measuring respectively in identical reaction temperature joined the iodine detection
Reaction time needed for the iodine standard serial solution of reagent reaches target absorbance value, and joined the iodine detection examination
Reaction time needed for the sample liquid of agent reaches target absorbance value, joined the iodine standard system of the iodine detection reagent
The reaction time of column solution establishes standard curve with corresponding iodine concentration, by the standard curve and joined the iodine inspection
Iodine content in sample liquid is calculated in the reaction time of the sample liquid of test agent.
The iodine standard serial solution of 3 different values is at least used, wherein the content of iodine is divided in iodine standard serial solution I
Not Wei 2,5,10,20,40,50,60,80,100,150,200,300ug/L, the content of iodine in iodine standard serial solution II
Respectively 50,100,200,300,400,600,800,1000,1200ug/L, the content of iodine in iodine standard serial solution III
Respectively 5,10,20,30,40,50,60,80,100mg/Kg.
Wherein iodine standard serial solution or sample liquid can choose following any side with reacting for iodine detection reagent
Method:
Method 1, accurately pipette iodine standard serial solution I and each 0.5-5ml of sample liquid or iodine standard serial solution II or
0.2-1ml digestion solution is added in test tube in person's iodine standard serial solution III and each 0.1-0.5ml of sample, shakes and mixes in test tube
Solution, shake in 2-10 minutes mixes, is added with digestion solution equivalent neutralizer, shake the solution mixed in test tube, 2-10 minutes
It shakes and mixes, the reducing agent with digestion solution equivalent is added, shake the solution mixed in test tube, the instruction with digestion solution equivalent is added
The solution mixed in test tube is shaken in agent, prepares timer, is added with digestion solution equivalent oxidant, starts timing, shakes and mix examination
Solution in pipe stands observation, when test tube solution becomes aubergine by indigo plant, stops timing, recording reacting time, or pass through
In iodine detector, the time of oxidant to the absorbance value for reaching setting is added as the reaction time in automatic detection.
Method 2: digestion solution is first added when reagent fills with method 1 in the adding amount of iodine standard serial solution and reagent,
The solution mixed in test tube is shaken, is shaken 1-30 minutes, neutralizer is added, shakes the solution mixed in test tube, shakes 1-30 points
Reducing agent is added in clock, shakes the solution mixed in test tube, stands 0-10 minutes, while indicator and oxidant is added, starts to count
When, the solution mixed in test tube is shaken, observation is stood, when test tube solution becomes aubergine by indigo plant, stops timing, record reaction
Time, or by the way that in iodine detector, indicator and oxidant is added to the absorbance value for reaching setting in automatic detection
Time is as the reaction time.
Method 3: the adding amount of iodine standard serial solution and reagent is with method 1, and when reagent fills, resolution is first added simultaneously
Liquid and neutralizer shake the solution mixed in test tube, shake 1-30 minutes, and reducing agent is added, and shake the solution mixed in test tube,
0-10 minutes are stood, indicator is added, shakes the solution mixed in test tube, stands 0-10 minutes, oxidant is added, starts to count
When, the solution mixed in test tube is shaken, observation is stood, when test tube solution becomes aubergine by indigo plant, stops timing, record reaction
Time, or by the way that in iodine detector, the time conduct of oxidant to the absorbance value for reaching setting is added in automatic detection
Reaction time.
Method 4: the adding amount of iodine standard serial solution and reagent is with method 1, and when reagent fills, resolution is first added simultaneously
Liquid and neutralizer shake the solution mixed in test tube, shake 1-30 minutes, and reducing agent is added, and shake the solution mixed in test tube,
0-10 minutes are stood, while indicator and oxidant is added, starts timing, shakes the solution mixed in test tube, stands observation, when
When test tube solution becomes aubergine by indigo plant, stop timing, recording reacting time, or pass through in iodine detector, it is automatic to examine
The time that indicator and oxidant to the absorbance value for reaching setting is added is surveyed as the reaction time.
Method 5: digestion solution is first added when reagent fills with method 1 in the adding amount of iodine standard serial solution and reagent,
The solution mixed in test tube is shaken, is shaken 1-30 minutes, neutralizer is added, shakes the solution mixed in test tube, shakes 1-30 points
Clock, while reducing agent, indicator and oxidant is added, start timing, shake the solution mixed in test tube, stands observation, work as examination
When pipe solution becomes aubergine by indigo plant, stop timing, recording reacting time, or pass through in iodine detector, it is automatic to detect
Reducing agent, indicator and oxidant is added to the time for the absorbance value for reaching setting as the reaction time.
Method 6: the adding amount of iodine standard serial solution and reagent is with method 1, and when reagent fills, resolution is first added simultaneously
Liquid and neutralizer shake 1-30 minutes, while reducing agent, indicator and oxidant are added, and start timing, shake and mix in test tube
Solution, stand observation, when test tube solution becomes aubergine by indigo plant, stop timing, recording reacting time, or first by iodine
In plain detector, the time of reducing agent, indicator and oxidant to the absorbance value for reaching setting is added as anti-in automatic detection
Between seasonable.
The calculation method of iodine content:
The calculation formula (see WS/T107-2016) that laboratory is announced is controlled according to national IDD(Iodine deficiency disorders), calculates linear regression
Related coefficient (r).
Absolute deviation=| yi-yiEstimated value | ... ... ... ... ... ...
(3)
In formula:
Xi-the theoretical concentration of measurement solution;
Yi-actual measured value corresponding with measurement solution concentration;
I -1,2,3 ... ..., n.
Dependence among equations absolute coefficient answers >=0.999.
The mass concentration of iodine in test sample is pressedCalculation formula are as follows:
S calculation formula are as follows:
CV calculation formula are as follows:
(4), (5), in (6) formula:
xi--- the concentration value (unit μ g/L) (i=1~10) of calibration object;
--- the average value of sample measurement concentration value;
S --- standard deviation;
N --- sample size (n=10);
CV --- the coefficient of variation;
Calibration curve method: the iodine concentration using iodine standard serial solution I or II or III is as abscissa and reaction time
Semilog ordinate draws standard curve in semilog coordinate system, is checked on standard curve with the reaction time of sample liquid
Iodine quality concentration in institute's sample, then the mass concentration by iodine in formula (4) calculating test sample.
The reaction time of 2 various concentration iodine of test example
When environment temperature is 25 degree, the iodine detection examination prepared in embodiment 1-3 and comparative example is respectively adopted
Agent is measured the reaction time of the iodine standard substance of various concentration, and the results are shown in Table 1.
The iodine standard substance of 1 various concentration of table uses the reaction time of different iodine detection reagents
Sulfuric acid in oxidant increases stability of the oxidant in metachromasia, so that reaction power regression curve
Time and detected value goodness of fit coefficient R value can achieve 0.9995 or more, meanwhile, so that the iodide ion of various concentration changes colour
Margi n pulls big between reaction time increases the detection sensitivity and accuracy of the iodide ion of high concentration so that an iodine from
Sub- detection range can achieve 1-2000 μ g/L.
The storage-stable of 3 iodine detection reagent of test example
The iodine detection reagent prepared in Example 1-3 and comparative example respectively carries out storage-stable experiment.
Sodium hydroxide is added in digestion solution, validity period and the stability of digestion solution can be improved, and is added in reducing agent
Sodium chloride increases validity period and the storage stability of reducing agent.
Iodine assay in 4 urine of test example
Iodine assay in urine is carried out with the iodine detection reagent 3-1 in embodiment 3, measures national standard object
Matter (standard substance Α definite value is 76.9ug/L ± 9, and standard substance B definite value is 232ug/L ± 10), iodine standard serial solution uses
50,100,200,300,400ug/L calibrations, measurement result are as shown in the table.
Measurement meets calibration value.
Iodine assay in 5 water of test example
Iodine assay in water is carried out with the iodine detection reagent 3-4 in embodiment 3, measures national standard substance
(standard substance Α definite value is 8.4ug/L ± 1.2, and standard substance B definite value is 55ug/L ± 6), iodine standard serial solution using 2,
5,10,20,40,60,80ug/L calibration, measurement result are as shown in the table.
Measurement meets calibration value.
Iodine assay in 6 salt of test example
Iodine assay in salt is carried out with the iodine detection reagent 3-1 in embodiment 3, measures national standard substance
(standard substance Α definite value is 11.3mg/Kg ± 2, and standard substance B definite value is 23.1mg/Kg ± 2), iodine standard serial solution uses
5,10,20,30,40mg/Kg calibrations, measured result are as follows.
Measurement meets calibration value.
Iodine assay in 7 blood of test example
Iodine assay in blood is carried out with the iodine detection reagent 3-5 in embodiment 3, due to currently without blood iodine
National standard substance, this reagents series detected using two parts of methods of inspection with people's blood sample on the same day and urine sample comparison,
As a result as follows.
Calibration object/sample ug/L | As a result |
Urine sample A | 135.1ug/L |
Urine sample A | 138.9ug/L |
Urine sample B | 248.6ug/L |
Urine sample B | 244.7ug/L |
Blood sample A | 140.8ug/L |
Blood sample A | 143.1ug/L |
Blood sample B | 241.7ug/L |
Blood sample B | 246.2ug/L |
Iodide determination result and the measurement result in urine sample are almost the same in blood sample.
National standard substance number and definite value in test example 4,5,6 is as follows:
Reference name | Number | Definite value |
Urinate iodine national standard substance A | GBW09108 | 76.9±9ug/L |
Urinate iodine national standard substance A | GBW09110 | 232±10ug/L |
Water iodine national standard substance A | GBW09113F | 8.4±1.2ug/L |
Water iodine national standard substance A | GBW09114F | 55±6ug/L |
Salt iodine national standard substance A | GBW10006V | 11.3±2mg/Kg |
Salt iodine national standard substance A | GBW10007V | 23.1±2mg/Kg |
It is added to sulfuric acid in oxidant in iodine detection reagent of the invention, increases oxidant in metachromasia
Stability so that reaction the power regression curve time and detected value goodness of fit coefficient R value can achieve 0.9995 or more, together
When, so that the margi n pulls big between the iodide ion metachromasia time of various concentration, increases the detection of the iodide ion of high concentration
Sensibility and accuracy, so that an iodide ion detection range can achieve 1-2000 μ g/L;Sodium hydroxide in digestion solution,
Validity period and the stability of digestion solution are improved, to increase validity period and the stabilization of iodine detection reagent of the invention
Property.Iodine detection reagent of the invention can be used for urine, water, in salt and blood iodine assay, measurement knot
Fruit meets calibration value, and measuring method is simple, and detection stability is good, and accuracy is high.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of iodine detection reagent, which is characterized in that including digestion solution, neutralizer, reducing agent, the indicator being retained separately
And oxidant;
The oxidant is the aqueous sulfuric acid of quadrivalent cerium, and the concentration of the quadrivalent cerium is 0.04~15mol/L, the sulfuric acid
Concentration is 0.05~9mol/L.
2. a kind of iodine detection reagent according to claim 1, which is characterized in that the digestion solution is that concentration is 0.07
The aqueous sodium hypochlorite solution of~0.6mol/L.
3. a kind of iodine detection reagent according to claim 1, which is characterized in that the digestion solution be sodium hypochlorite and
The concentration of the aqueous solution of sodium hydroxide, the sodium hypochlorite and the sodium hydroxide be respectively 0.07~0.6mol/L and 0.1~
2.5mol/L。
4. a kind of iodine detection reagent according to claim 1, which is characterized in that the quadrivalent cerium be Cericammoniumsulfate or
One or both of cerous sulfate.
5. a kind of iodine detection reagent according to any one of claims 1 to 4, which is characterized in that the neutralizer is
One or more of sulfuric acid solution, hydrochloric acid solution, perchloric acid solution or sodium chlorate solution, the pH value of the neutralizer is less than 3.
6. a kind of iodine detection reagent according to any one of claims 1 to 4, which is characterized in that the reducing agent is
Concentration is the sodium arsenite aqueous solution of 0.05~1mol/L.
7. a kind of iodine detection reagent according to any one of claims 1 to 4, which is characterized in that the reducing agent is
The concentration of the aqueous solution of sodium arsenite and sodium chloride, the sodium arsenite and sodium chloride be respectively 0.05~1mol/L and 0.01~
2mol/L。
8. a kind of iodine detection reagent according to any one of claims 1 to 4, which is characterized in that the indicator is
The aqueous sulfuric acid of Ferroin reagent, the concentration of Phen is 0.005~1.6mol/L, ferrous ion in the indicator
Concentration be 0.003~1.5mol/L, the concentration of sulfuric acid is 0.01~1.5mol/L.
9. a kind of iodine detection reagent according to claim 8, which is characterized in that it is sub- that the ferrous ion is selected from sulfuric acid
One or more of iron, iron ammonium sulfate or frerrous chloride.
10. the method that a kind of application such as described in any item iodine detection reagents of claim 1-9 carry out iodine detection,
It is characterized in that, takes iodine standard serial solution and sample liquid, measuring respectively in identical reaction temperature joined the iodine inspection
Reaction time needed for the iodine standard serial solution of test agent reaches target absorbance value, and joined the iodine detection
Reaction time needed for the sample liquid of reagent reaches target absorbance value, joined the iodine standard of the iodine detection reagent
The reaction time of serial solution establishes standard curve with corresponding iodine concentration, by the standard curve and joined the iodine
Iodine content in sample liquid is calculated in the reaction time of the sample liquid of detection reagent.
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