CN101625316A - Method for detecting phosphorus content in phosphorylated polysaccharide - Google Patents
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Abstract
The invention relates to a method for detecting the phosphorus content in phosphorylated polysaccharide. The method comprises the following steps: preparing a phosphate radical gradient standard solution, adopting distilled water as a blank comparison to replace the standard solution and processing according to the same condition; and then detecting a light absorbing value in the position of 824 nm, drawing a standard curve and establishing a regression equation; then after the phosphorylated polysaccharide to be detected is processed, neutralizing by mixed acid and diluting and fixing volume to prepare a sample solution; processing the sample solution having the same volume with the processed phosphate gradient standard solution under the same condition and detecting the light absorbing value; calculating the phosphate radical concentration of the sample solution to be detected according to the regression equation and further confirming the phosphorus content of the phosphorylated polysaccharide to be detected. The method has shorter detecting time, small repeated detection error, wider detecting range, accurate and reliable result and low detecting cost and is easy for generalization and implementation.
Description
Technical field
The present invention relates to a kind of method of measuring phosphorus content, be specifically related to a kind of method of measuring phosphorus content in the phosphorylated polysaccharide.
Technical background
The various vital movements of polysaccharide wide participation cell and have the various biological function as enhance immunity characteristic, antitumor, antiviral, anticoagulation, delay senility etc., thereby are subjected to people's generally attention, are researched and developed accordingly.But the activity of polysaccharide is subjected to the restriction of its structure directly or indirectly, therefore, takes certain method that polysaccharide structures is suitably modified and is necessary.
Phosphorus is the more element of people's in-vivo content, not only participates in constituting soft tissues such as bone, tooth and nerve fiber, also participates in some the important metabolic processes in the body.Second messenger's cyclic adenosine monophosphate, cyclic guanylic acid etc. are the compounds of phosphorous-containigroups groups in nucleic acid, phosphoprotein, phosphatidase and the cell.Synthetic, the decomposition of high energy phosphate compound are the main modes of body utilization, storage power, and the generation of all energy in the body stores and all depends on an amount of phosphorus supply.Hypophosphatemia can appear in the phosphorus shortage, shows as anaemia, myasthenia, ostalgia, osteomalacia, asthenia universalis, so that neural, insanity.
Phosphorylated polysaccharide is that P elements is with the hydroxyl on the form substituted polysaccharide of phosphate radical.Phosphorylated polysaccharide has kept the basic configuration of polysaccharide, makes the saccharide compound of some these non-activities have activity simultaneously, or significantly improves the biologically active of some polysaccharide.Studies show that, biologically actives such as phosphorylated polysaccharide has antitumor, antiviral, antibiotic and immunomodulator, its activity generally is higher than polysaccharide, and to be easier to be that body absorbs and utilizes.
The existing method of measuring phosphorus content has: neutron activation analysis method (INAA), atomic emission spectrometry (AES), atomic absorption spectrography (AAS) (AAS), inductively coupled plasma mass spectrometry method (ICP-MS), ultraviolet spectrophotometry and fluorescence spectrophotometry, electrochemical methods etc.Chinese patent CN 101251489A discloses " a kind of rapid preprocessing method of measuring total phosphorus content in the sediment " on August 27th, 2008, soil sample is cleared up the back add developer, measures at the 700nm place.Chinese patent CN 1991339A discloses " method of total phosphorus content in a kind of analytic sample " on July 4th, 2007, testing sample is mixed with a kind of distintegrant, dissolve fully with a kind of acid solution again, be reduced into the phosphorus molybdenum blue, utilize the phosphorus molybdenum blue to have the maximum light absorption value to measure at the 710nm place, the absorbance scope that records is 0.3～0.7.Chinese patent CN1296173A discloses " assay method of content of inorganic phosphorus in the phosphorous antistatic agent " May 23 calendar year 2001, and the Phos in the antistatic agent is extracted with saturated sodium nitrate, clears up the back and carries out colorimetric estimation with phosphorus molybdenum Huang at the 420nm place.In the above method, the disposal route of sample just be suitable at sample, the scope of application is little, the detection limit and the range of linearity of clearly measuring not, thereby cause its range of application narrow.Document " researchs of lentinan phosphorylation modification process conditions " (" food and fermentation industries ", 2007,33 (12), 64～67) reported the method for measuring phosphorus content in the lentinan phosphate in " food and fermentation industries " the 12nd phase in 2007, sample preparation adopts ashing method, and the processing time is long, process is loaded down with trivial details, ashing composition dissolubility is bad, and whole process easily causes measurement result inaccurate based on subjective judgement.Chinese patent CN 1635366A discloses " a kind of method of utilizing the low resolution icp ms to detect phosphorus " on July 6th, 2005, the method is measured the concentration of phosphorus indirectly by the oxide concentration of measuring phosphorus, is difficult to popularize but testing cost is too high.For the method for measuring phosphorus content in the phosphorylated polysaccharide, people expect to have a kind of accuracy height, good reproducibility, cost is low and the assay method that is easy to promote.
Summary of the invention
Technical matters to be solved by this invention provides the method for phosphorus content in the high mensuration phosphorylated polysaccharide of a kind of good reproducibility, accuracy.
For solving the problems of the technologies described above, a kind of method of measuring phosphorus content in the phosphorylated polysaccharide of the present invention comprises the steps:
(1) drawing standard curve and set up regression equation: the NaH that gets certain mass
2PO
4Constant volume prepares phosphate radical (PO in volumetric flask
4 3-) concentration is the mother liquor of 10ug/ml, dilute the phosphate radical gradient standard solution of preparation 0.2,0.5,1,2,3,4,5,7,9,10ug/ml more successively, get above-mentioned gradient standard solution 3～5ml respectively, adding 1.8～3ml pH value is 7.0 Tris damping fluid, shaking up back adding 1.2～2ml concentration is the aqueous ascorbic acid of 125mg/ml, leaves standstill 1～2min and adds the H that 1.8～3ml concentration is 1mol/L afterwards successively
2SO
4With 0.6～1ml concentration be the ammonium molybdate solution of 30mg/ml, mix the back and in 30～45 ℃ thermostat water bath, be incubated 20～30min, replace described standard solution to handle by similarity condition with distilled water as blank, measuring absorbance value at the 824nm place respectively then (is the OD value, optical density), with the phosphate concentration is horizontal ordinate (X), and absorbance value is ordinate (Y), and the drawing standard curve is also set up regression equation;
(2) processing of sample: in constant temperature oven, the phosphorylated polysaccharide testing sample is handled 30～45min down at 50～60 ℃ and remove residual moisture, take by weighing the above-mentioned dry sample of certain mass, add nitration mixture, wherein the ratio of sample and nitration mixture is, weight: volume=1～2.5mg: 1ml, the volume parts of each composition is than being HNO in the described nitration mixture
3: HClO
4=4: 1, the static back of spending the night is cleared up 1～2 hour to the solution clarification in 120 ℃, get digestion solution A;
(3) mensuration of phosphorus content: with digestion solution A at 40～60 ℃, 0.06 the concentrating under reduced pressure evaporate to dryness obtains dry B under the～0.08MPa, dry B constant volume is prepared into B solution in volumetric flask, make its phosphate concentration in 0.2～10ug/ml scope, get with step (1) in gradient standard solution equal volume described B solution and according to with step (1) in identical condition handle, promptly get B solution 3～5ml, join 1.8～3ml pH value and be in 7.0 the Tris damping fluid, shaking up back adding 1.2～2ml concentration is the aqueous ascorbic acid of 125mg/ml, leaves standstill 1～2min and adds the H that 1.8～3ml concentration is 1mol/L afterwards successively
2SO
4With 0.6～1ml concentration be the ammonium molybdate solution of 30mg/ml, in 30～45 ℃ thermostat water bath, be incubated 20～30min after mixing, replace described B solution to handle by similarity condition with distilled water as blank, measure absorbance value then at the 824nm place, three absorbance values of each sample determination, get the regression equation of being set up in its mean value substitution step (1), calculate the phosphate concentration (ug/ml) of sample solution behind the constant volume; Then, volume (ml) according to the sample solution of institute's constant volume is calculated phosphate content (ug) in the constant volume sample B of the institute solution, calculate the content (ug/mg) of the phosphate radical in the phosphorylated polysaccharide dry of surveying again according to the weight (mg) of used phosphorylated polysaccharide dry sample, at last, calculate the phosphorus content (ug/mg) of the phosphorylated polysaccharide of surveying according to the content of phosphorus in phosphate radical.
Table 1 is the data of embodiment 1～3 typical curve, Fig. 1～3 are the typical curve that light absorption among the embodiment 1～3 (OD) value (Y) is drawn gradient phosphate radical concentration of standard solution (X), set up its corresponding regression equation, its coefficient R respectively according to the data of embodiment 1～3 drawing standard curve
2Value all is in close proximity to 1, illustrates that its corresponding regression equation all has utmost point significant linear relationship.
Each the pairing light absorption of gradient phosphate radical standard solution (OD) value among table 1 embodiment 1～3
| Gradient phosphate radical concentration of standard solution (ug/ml) | The embodiment 1 OD value of surveying | The |
The embodiment 3 OD value of surveying |
| ??0.2 | ??0.0258 | ??0.0258 | ??0.0260 |
| ??0.5 | ??0.0638 | ??0.0638 | ??0.0640 |
| ??1 | ??0.1321 | ??0.1314 | ??0.1327 |
| ??2 | ??0.2517 | ??0.2518 | ??0.2519 |
| ??3 | ??0.3811 | ??0.3810 | ??0.3811 |
| ??4 | ??0.4963 | ??0.4962 | ??0.4963 |
| ??5 | ??0.6285 | ??0.6285 | ??0.6288 |
| ??7 | ??0.8900 | ??0.8899 | ??0.8901 |
| ??9 | ??1.1371 | ??1.1372 | ??1.1376 |
| ??10 | ??1.2658 | ??1.2657 | ??1.2667 |
| ??R 2 | ??0.9999 | ??0.9999 | ??0.9999 |
Table 2 has provided at the phosphorus content of same sample copy inventive embodiments mensuration and the comparison of the phosphorus content data that ICP (inductively coupled plasma emission spectrography) measures; ICP mensuration herein is in other mechanism for testing mensuration, and it is relatively more accurate, reliable at present assay method that ICP measures, but is difficult to popularize because of testing expense is higher.The measurement result of the embodiment of the invention and ICP measurement result basically identical illustrate that measurement result of the present invention is accurately, reliably.
Phosphorus content (ug/mg) result that table 2 embodiment of the invention is measured the corresponding phosphorylated polysaccharide dry sample of measuring with ICP compares
| The embodiment sample | The phosphorus content of this method working sample (ug/mg) | The phosphorus content of ICP working sample (ug/mg) |
| Embodiment 1 sample | ??15.50 | ??14.98 |
| |
??74.07 | ??71.10 |
| Embodiment 3 samples | ??114.86 | ??120.60 |
The invention has the beneficial effects as follows: a kind of method of measuring phosphorus content in the phosphorylated polysaccharide of the present invention, do not comprise the pretreated time of Specimen eliminating, the time that sample is once measured only be about 30 minutes and repeated detection error little, the setting-out line scope is 0.2～10ug/ml, detect and be limited to 0.05ug/ml, overcome measure in the phosphorus content method in the past the sample scope of application little, restricted big, cost is high, and shortcomings such as measurement result is inaccurate, poor repeatability.Method testing result of the present invention accurately and reliably, good reproducibility, cost of determination is low, is easy to promotion and implementation.
Description of drawings
Below in conjunction with the drawings and specific embodiments the present invention is described in further detail:
Fig. 1 is the typical curve according to data creating among the embodiment 1;
Fig. 2 is the typical curve according to data creating among the embodiment 2;
Fig. 3 is the typical curve according to data creating among the embodiment 3.
Embodiment
Embodiment 1
The invention provides a kind of method of measuring phosphorus content in the phosphorylated polysaccharide, concrete steps are as follows:
(1) drawing standard curve and set up regression equation: get 12.63mg NaH
2PO
4Constant volume prepares phosphate concentration in the 1000ml volumetric flask be the mother liquor of 10ug/ml, dilute the phosphate radical gradient standard solution of preparation 0.2,0.5,1,2,3,4,5,7,9,10ug/ml more successively, measure above-mentioned standard solution 3ml respectively, adding 1.8ml pH value is 7.0 Tris damping fluid, shaking up back adding 1.2ml concentration is the aqueous ascorbic acid of 125mg/ml, leaves standstill 2min and adds the H that 1.8ml concentration is 1mol/L afterwards successively
2SO
4With 0.6ml concentration be the ammonium molybdate solution of 30mg/ml, mix the back and in 30 ℃ thermostat water bath, be incubated 30min, replace described standard solution to handle by similarity condition with distilled water as blank, measure light absorption (OD) value (result is as shown in table 1) then respectively at the 824nm place, with the phosphate concentration is that horizontal ordinate (X), absorbance value are ordinate (Y) drawing standard curve (as Fig. 1), obtain regression equation: Y=0.1264X+0.0002, R=0.9999;
(2) processing of sample: in constant temperature oven testing sample is handled 30min down at 60 ℃ and remove residual moisture, take by weighing the above-mentioned sample of 2mg, add nitration mixture 2ml, the volume parts of each composition is than being HNO in the described nitration mixture
3: HClO
4=4: 1, the static back of spending the night is cleared up 2 hours to the solution clarification in 120 ℃, get digestion solution A;
(3) mensuration of phosphorus content: digestion solution A concentrating under reduced pressure evaporate to dryness under 40 ℃, 0.08MPa is obtained dry B, dry B constant volume is made B solution in the 100ml volumetric flask, get B solution 3ml, add 1.8ml pH value and be in 7.0 the Tris damping fluid, shaking up back adding 1.2ml concentration is the aqueous ascorbic acid of 125mg/ml, leaves standstill 2min and adds the H that 1.8ml concentration is 1mol/L afterwards successively
2SO
4With 0.6ml concentration be the ammonium molybdate solution of 30mg/ml, in 30 ℃ thermostat water bath, be incubated 30min after mixing, replace described B solution to handle by similarity condition with distilled water as blank, measure absorbance value then at the 824nm place, each sample determination three times, the regression equation of being set up in mean value (Y) the 0.1200 substitution step (1) with institute's test sample product absorbance value (Y=0.1264X+0.0002) calculates behind the constant volume that phosphate concentration (X) is 0.95ug/ml in the sample B solution, calculate wherein phosphate content 95.00ug according to the sample B liquor capacity 100ml of institute's constant volume again, calculate the content 47.50ug/mg of the dry phosphorylated polysaccharide phosphate radical of surveying according to the weight 2mg of dry phosphorylated polysaccharide, according to phosphorus at phosphate radical (PO
4 3-) in content (about 32.63%) calculate the phosphorus content 15.50ug/mg of phosphorylated polysaccharide.
The invention provides a kind of method of measuring phosphorus content in the phosphorylated polysaccharide, concrete steps are as follows:
(1) drawing standard curve and set up regression equation: get 12.63mg NaH
2PO
4Constant volume prepares phosphate concentration in the 1000ml volumetric flask be the mother liquor of 10ug/ml, successively the phosphate radical gradient standard solution of dilution preparation 0.2,0.5,1,2,3,4,5,7,9,10ug/ml.Measure above-mentioned standard solution 5ml respectively, adding 3ml pH value is 7.0 Tris damping fluid, and shaking up back adding 2ml concentration is the aqueous ascorbic acid of 125mg/ml, leaves standstill 2min and adds the H that 3ml concentration is 1mol/L afterwards successively
2SO
4With 1ml concentration be the ammonium molybdate solution of 30mg/ml, mix the back and in 30 ℃ thermostat water bath, be incubated 45min, replace described standard solution to handle by similarity condition with distilled water as blank, measure light absorption (OD) value (result is as shown in table 1) then respectively at the 824nm place, with the phosphate concentration is horizontal ordinate (X), and absorbance value is ordinate (Y), drawing standard curve (as Fig. 2), obtain regression equation: Y=0.1264X+3E-6, R=0.9999;
(2) processing of sample: in constant temperature oven testing sample is handled 45min down at 50 ℃ and remove residual moisture, take by weighing the above-mentioned sample of 4mg, add nitration mixture 2ml, the volume parts of each composition is than being HNO in the described nitration mixture
3: HClO
4=4: 1, the static back of spending the night is cleared up 1.5 hours to the solution clarification in 120 ℃, get digestion solution A;
(3) mensuration of phosphorus content: digestion solution A concentrating under reduced pressure evaporate to dryness under 50 ℃, 0.07MPa is obtained dry B, with dry B constant volume in the 200ml volumetric flask, measure the B solution 5ml behind the constant volume, add 3ml pH value and be in 7.0 the Tris damping fluid, shaking up back adding 2ml concentration is the aqueous ascorbic acid of 125mg/ml, leaves standstill 2min and adds the H that 3ml concentration is 1mol/L afterwards successively
2SO
4With 1ml concentration be the ammonium molybdate solution of 30mg/ml, in 45 ℃ thermostat water bath, be incubated 20min after mixing, replace described B solution to handle by similarity condition with distilled water as blank, measure absorbance value then at the 824nm place, each sample determination three times, the concentration that the regression equation of being set up in mean value (Y) the 0.5740 substitution step (1) with institute's test sample product absorbance value (Y=0.1264X+3E-6) is calculated the phosphate radical in the sample solution behind the constant volume is 4.54ug/ml, volume 200ml according to the sample solution of institute's constant volume calculates phosphate content 908.00ug in the constant volume sample liquid again, calculate the content 227.00ug/mg of the dry phosphorylated polysaccharide phosphate radical of surveying according to the weight 4mg of dry phosphorylated polysaccharide, according to phosphorus at phosphate radical (PO
4 3-) in content (about 32.63%) calculate the phosphorus content 74.07ug/mg of phosphorylated polysaccharide.
Embodiment 3
The invention provides a kind of method of measuring phosphorus content in the phosphorylated polysaccharide, concrete steps are as follows:
(1) drawing standard curve and set up regression equation: get 12.63mg NaH
2PO
4Constant volume prepares phosphate concentration in the 1000ml volumetric flask be the mother liquor of 10ug/ml, successively the phosphate radical gradient standard solution of dilution preparation 0.2,0.5,1,2,3,4,5,7,9,10ug/ml.Measure above-mentioned standard solution 4ml respectively, adding 2.4ml pH value is 7.0 Tris damping fluid, and shaking up back adding 1.6ml concentration is the aqueous ascorbic acid of 125mg/ml, leaves standstill 2min and adds the H that 2.4ml concentration is 1mol/L afterwards successively
2SO
4With 0.8ml concentration be the ammonium molybdate solution of 30mg/ml, mix the back and in 40 ℃ thermostat water bath, be incubated 25min, handle by similarity condition as blank to replace described standard solution with distilled water, measure light absorption (OD) value (result is as shown in table 1) then respectively at the 824nm place, with the phosphate concentration is horizontal ordinate (X), and absorbance value is ordinate (Y), drawing standard curve (as Fig. 3), obtain regression equation: Y=0.1264X+0.0003, R=0.9999;
(2) processing of sample: in constant temperature oven testing sample is handled 40min down at 55 ℃ and remove residual moisture, take by weighing the above-mentioned sample of 10mg, add nitration mixture 4ml, the volume parts of each composition is than being HNO in the described nitration mixture
3: HClO
4=4: 1, the static back of spending the night is cleared up 1 hour to the solution clarification in 120 ℃, get digestion solution A;
(3) mensuration of phosphorus content: digestion solution A concentrating under reduced pressure evaporate to dryness under 60 ℃, 0.06MPa is obtained dry B, with dry B constant volume in the 500ml volumetric flask, measure the B solution 4ml behind the constant volume, add 2.4ml pH value and be in 7.0 the Tris damping fluid, shaking up back adding 1.6ml concentration is the aqueous ascorbic acid of 125mg/ml, leaves standstill 2min and adds the H that 2.4ml concentration is 1mol/L afterwards successively
2SO
4With 0.8ml concentration be the ammonium molybdate solution of 30mg/ml, in 40 ℃ thermostat water bath, be incubated 25min after mixing, replace described B solution to handle by similarity condition with distilled water as blank, measure absorbance value then at the 824nm place, each sample determination three times, the regression equation of being set up in mean value (Y) the 0.8900 substitution step (1) with institute's test sample product absorbance value (Y=0.1264X+0.0003) calculates that the phosphate concentration (X) in the sample solution is 7.04ug/ml behind the constant volume, volume 500ml according to the sample solution of institute's constant volume calculates phosphate content 3520ug in the constant volume sample liquid again, calculate the content 352ug/mg of the dry phosphorylated polysaccharide phosphate radical of surveying according to the weight 10mg of dry phosphorylated polysaccharide, according to phosphorus at phosphate radical (PO
4 3-) in content (about 32.63%) calculate the phosphorus content 114.86ug/mg of phosphorylated polysaccharide.
Claims (1)
1, a kind of method of measuring phosphorus content in the phosphorylated polysaccharide is characterized in that may further comprise the steps:
(1) drawing standard curve and set up regression equation: the NaH that gets certain mass
2PO
4Constant volume prepares the mother liquor that phosphate concentration is 10ug/ml in volumetric flask, dilute the phosphate radical gradient standard solution of preparation 0.2,0.5,1,2,3,4,5,7,9,10ug/ml more successively, get above-mentioned gradient standard solution 3～5ml respectively, adding 1.8～3ml pH value is 7.0 Tris damping fluid, shaking up back adding 1.2～2ml concentration is the aqueous ascorbic acid of 125mg/ml, leaves standstill 1～2min and adds the H that 1.8～3ml concentration is 1mol/L afterwards successively
2SO
4With 0.6～1ml concentration be the ammonium molybdate solution of 30mg/ml, mix the back and in 30～45 ℃ thermostat water bath, be incubated 20～30min, replace described standard solution to handle by similarity condition with distilled water as blank, measure absorbance value then at the 824nm place, with the phosphate concentration is horizontal ordinate, absorbance value is an ordinate, and the drawing standard curve is also set up regression equation;
(2) processing of sample: in constant temperature oven, the phosphorylated polysaccharide testing sample is handled 30～45min down at 50～60 ℃ and remove residual moisture, take by weighing the above-mentioned dry sample of certain mass, add nitration mixture, wherein the ratio of sample and nitration mixture is, weight: volume=1～2.5mg: 1ml, the volume parts of each composition is than being HNO in the described nitration mixture
3: HClO
4=4: 1, the static back of spending the night is cleared up 1～2 hour to the solution clarification in 120 ℃, get digestion solution A;
(3) mensuration of phosphorus content: with digestion solution A at 40～60 ℃, 0.06 the concentrating under reduced pressure evaporate to dryness obtains dry B under the～0.08MPa, dry B constant volume is prepared into B solution in volumetric flask, make its phosphate concentration in 0.2～10ug/ml scope, get with step (1) in gradient standard solution equal volume described B solution and according to with step (1) in identical condition handle, promptly get B solution 3～5ml, join 1.8～3ml pH value and be in 7.0 the Tris damping fluid, shaking up back adding 1.2～2ml concentration is the aqueous ascorbic acid of 125mg/ml, leaves standstill 1～2min and adds the H that 1.8～3ml concentration is 1mol/L afterwards successively
2SO
4With 0.6～1ml concentration be the ammonium molybdate solution of 30mg/ml, in 30～45 ℃ thermostat water bath, be incubated 20～30min after mixing, replace described B solution to handle by similarity condition with distilled water as blank, measure absorbance value then at the 824nm place, three absorbance values of each sample determination, get the regression equation of being set up in its mean value substitution step (1), calculate the phosphate concentration of sample solution behind the constant volume; Then, volume according to the sample solution of institute's constant volume is calculated phosphate content in the constant volume sample B of the institute solution, calculate the content of the phosphate radical in the phosphorylated polysaccharide dry of surveying again according to the weight of used phosphorylated polysaccharide dry sample, calculate the phosphorus content of the phosphorylated polysaccharide of surveying at last according to the content of phosphorus in phosphate radical.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101799459A (en) * | 2010-03-31 | 2010-08-11 | 天水师范学院 | Method for measuring phosphorus content of polysaccharide phosphate ester |
| CN101915814A (en) * | 2010-07-27 | 2010-12-15 | 中国蓝星（集团）股份有限公司 | Method for detecting azoisobutyronitrile residue in acrylonitrile polymerization solution |
| CN104483281A (en) * | 2014-12-30 | 2015-04-01 | 金堆城钼业股份有限公司 | Rapid analysis method for rhenium in low-rhenium high sulfate radical waste liquid |
-
2009
- 2009-08-05 CN CN200910162002XA patent/CN101625316B/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101799459A (en) * | 2010-03-31 | 2010-08-11 | 天水师范学院 | Method for measuring phosphorus content of polysaccharide phosphate ester |
| CN101915814A (en) * | 2010-07-27 | 2010-12-15 | 中国蓝星（集团）股份有限公司 | Method for detecting azoisobutyronitrile residue in acrylonitrile polymerization solution |
| CN104483281A (en) * | 2014-12-30 | 2015-04-01 | 金堆城钼业股份有限公司 | Rapid analysis method for rhenium in low-rhenium high sulfate radical waste liquid |
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