CN113311100A - Method for measuring lanthanum content in lanthanum carbonate preparation - Google Patents
Method for measuring lanthanum content in lanthanum carbonate preparation Download PDFInfo
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- CN113311100A CN113311100A CN202110581470.1A CN202110581470A CN113311100A CN 113311100 A CN113311100 A CN 113311100A CN 202110581470 A CN202110581470 A CN 202110581470A CN 113311100 A CN113311100 A CN 113311100A
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- lanthanum
- lanthanum carbonate
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- ion chromatography
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- 229910017569 La2(CO3)3 Inorganic materials 0.000 title claims abstract description 37
- NZPIUJUFIFZSPW-UHFFFAOYSA-H lanthanum carbonate Chemical compound [La+3].[La+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O NZPIUJUFIFZSPW-UHFFFAOYSA-H 0.000 title claims abstract description 37
- 229960001633 lanthanum carbonate Drugs 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 26
- 229910052746 lanthanum Inorganic materials 0.000 title claims abstract description 19
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 150000002500 ions Chemical class 0.000 claims abstract description 15
- 238000004255 ion exchange chromatography Methods 0.000 claims abstract description 14
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 9
- 239000012488 sample solution Substances 0.000 claims abstract description 9
- 239000000523 sample Substances 0.000 claims abstract description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000012417 linear regression Methods 0.000 claims abstract description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 4
- 238000004458 analytical method Methods 0.000 claims abstract description 3
- 238000011084 recovery Methods 0.000 claims description 7
- 230000035945 sensitivity Effects 0.000 abstract description 5
- 238000001514 detection method Methods 0.000 description 5
- 208000020832 chronic kidney disease Diseases 0.000 description 4
- 201000005991 hyperphosphatemia Diseases 0.000 description 4
- 208000028208 end stage renal disease Diseases 0.000 description 3
- 201000000523 end stage renal failure Diseases 0.000 description 3
- 238000000502 dialysis Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011002 quantification Methods 0.000 description 2
- 102000006335 Phosphate-Binding Proteins Human genes 0.000 description 1
- 108010058514 Phosphate-Binding Proteins Proteins 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- MWKXCSMICWVRGW-UHFFFAOYSA-N calcium;phosphane Chemical compound P.[Ca] MWKXCSMICWVRGW-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 208000022831 chronic renal failure syndrome Diseases 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 229940099065 fosrenol Drugs 0.000 description 1
- 210000001035 gastrointestinal tract Anatomy 0.000 description 1
- 238000001631 haemodialysis Methods 0.000 description 1
- 230000000322 hemodialysis Effects 0.000 description 1
- 208000017169 kidney disease Diseases 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000002085 persistent effect Effects 0.000 description 1
- 238000005220 pharmaceutical analysis Methods 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/96—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation using ion-exchange
Abstract
The invention discloses a method for measuring lanthanum content in a lanthanum carbonate preparation, which comprises the following steps: preparing lanthanum carbonate linear control solutions with different concentrations, respectively injecting the lanthanum carbonate linear control solutions into ion chromatography, and carrying out ion chromatography analysis, wherein the ion chromatography conditions are as follows: eluting with 5mM nitric acid solution at flow rate of 0.4ml/min, column temperature of 30 deg.C, and running time of 8 min; calculating linear regression by taking the concentrations of different solutions as horizontal coordinates and peak areas as vertical coordinates, and establishing a standard curve to obtain a regression equation; preparing 1000ug/ml of lanthanum carbonate sample solution, injecting the lanthanum carbonate sample solution into an ion chromatograph, carrying out ion chromatographic analysis, and calculating the lanthanum content in the sample by adopting a standard curve method. The invention has high automation degree and is easy to realize batch sample introduction; the method has the advantages of rapidness, convenience, good repeatability, high sensitivity and the like.
Description
Technical Field
The invention relates to a method for measuring lanthanum content in a lanthanum carbonate preparation, and belongs to the technical field of pharmaceutical analysis.
Background
Hyperphosphatemia is one of the important complications of end-stage renal failure, and 80% of renal dialysis patients suffer from this disease. Studies have shown that in end-stage renal failure patients, the persistent increase in calcium phosphorus product and hyperphosphatemia is directly proportional to the mortality of the patient. Therefore, the control of hyperphosphatemia has important significance for improving the life quality of the end-stage renal failure patients and reducing the death rate.
Lanthanum carbonate (Fosrenol) is a novel phosphorus binder developed by charle (shire) of the uk for the treatment of hyperphosphatemia in chronic renal failure patients undergoing hemodialysis or continuous ambulatory peritoneal dialysis. It has the advantages of fast phosphate binding speed, large amount, no absorption in gastrointestinal tract, low accumulation in body tissue, high tolerance, etc. and is one new kind of medicine with high phosphotungemia treating effect in nephropathy.
Lanthanum belongs to rare metals, the literature method is few, the literature method for measuring the lanthanum content mostly adopts the classical volumetric method (titration method), the photometric method and the like, the operation steps are long and time-consuming, a plurality of chemical reagents are required in the process, the sensitivity is low, and the interference is easy to occur.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of the prior art and provides the method for measuring the lanthanum content in the lanthanum carbonate preparation, which has high automation degree and is easy to realize batch sample introduction; the method has the advantages of rapidness, convenience, good repeatability, high sensitivity and the like.
In order to solve the technical problem, the invention provides a method for measuring lanthanum content in a lanthanum carbonate preparation, which comprises the following steps:
preparing lanthanum carbonate linear control solutions with different concentrations, respectively injecting the lanthanum carbonate linear control solutions into ion chromatography, and carrying out ion chromatography analysis, wherein the ion chromatography conditions are as follows: eluting with 5mM nitric acid solution at flow rate of 0.4ml/min, column temperature of 30 deg.C, and running time of 8 min;
calculating linear regression by taking the concentrations of different solutions as horizontal coordinates and peak areas as vertical coordinates, and establishing a standard curve to obtain a regression equation;
preparing 1000ug/ml of lanthanum carbonate sample solution, injecting the lanthanum carbonate sample solution into an ion chromatograph, carrying out ion chromatographic analysis, and calculating the lanthanum content in the sample by adopting a standard curve method.
Preferably, the concentration of the lanthanum carbonate linear control solution is 400ug/ml, 600ug/ml, 800ug/ml, 1000ug/ml, 1200ug/ml respectively.
Preferably, the ion chromatography uses a universal ion chromatograph-930, and the chromatographic column is a C4 guard column 150mm x 4.0 um.
Preferably, the resulting standard curve is y-13.001 x +0.6471 with a correlation coefficient R of 0.9999.
Preferably, the concentration of the solution for limiting the quantification of the ion chromatographic analysis is 2.8ug/ml, and the concentration of the solution for limiting the detection is 0.9 ug/ml.
Preferably, the recovery rate of the sample solution of lanthanum carbonate is between 98% and 102%; the RSD of the recovery rate (N ═ 9) was 1.55.
The invention achieves the following beneficial effects: the invention has high automation degree and is easy to realize batch sample introduction; fast, convenient, good in repeatability and high in sensitivity.
Drawings
FIG. 1 is an ion chromatogram for determination of lanthanum content at a concentration of 1mg/ml in example 1.
Detailed Description
The present invention will be further described with reference to the following examples. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
Example 1
Preparing lanthanum carbonate linear control solutions (400ug/ml, 600ug/ml, 800ug/ml, 1000ug/ml and 1200ug/ml), respectively injecting the solutions into an ion chromatograph, and performing chromatographic analysis under the following conditions:
equipment: wantong ion chromatograph-930 (919 automatic sample injector)
A chromatographic column: c4 protection (150mm x 4.0um)
Eluent: 5mM nitric acid solution
Flow rate: 0.4ml/min
Column temperature: 30 deg.C
Operating time: and 8 min.
Taking the concentration of the solution as a horizontal coordinate and the peak area as a vertical coordinate, calculating linear regression, establishing a standard curve, and obtaining a regression equation as shown in table 1:
table 1: results of the Linear and Range experiments
As can be seen from Table 1, the Relative Standard Deviation (RSD) of the peak area of 3 needles at each linearity level is not more than 10%; the obtained standard curve is that y is 13.001x +0.6471, the correlation coefficient R is 0.9999, and the lanthanum carbonate is in good linear relation within 400ug/ml-1200 ug/ml.
FIG. 1 is an ion chromatogram for determination of lanthanum content at a concentration of 1mg/ml in this example.
Example 2
According to the signal-to-noise ratio of the 1mg/ml solution in example 1, the quantitative limiting solution with the signal-to-noise ratio of about 10 was diluted, the quantitative limiting solution was diluted 3 times to be the detection limiting solution, and the solutions were injected into the ion chromatography, respectively, and subjected to the chromatographic analysis, and the quantitative limit and the detection limit concentrations were calculated, the results are shown in table 2:
table 2: experimental results of detection limit and quantitative limit
As shown in Table 2, the method has a detection limit concentration of 0.9ug/ml and a quantification limit concentration of 2.8ug/ml, and has high sensitivity.
Example 3
Lanthanum carbonate accuracy solutions (800ug/ml, 1000ug/ml, 1200ug/ml) were prepared, injected into ion chromatography, and subjected to chromatographic analysis, and the recovery rate was calculated by a standard curve method, with the results shown in table 3:
table 3: accuracy experimental results
As can be seen from Table 3, the recovery rate of lanthanum carbonate in each sample solution at each concentration is between 98% and 102%; RSD1.55 for recovery (N ═ 9) with good accuracy.
Example 4
Preparing a lanthanum carbonate solution 1mg/ml, injecting the lanthanum carbonate solution into an ion chromatograph, performing chromatographic analysis, calculating 6-needle repeatability RSD, establishing a system by another experimenter on another date, preparing a lanthanum carbonate solution 1mg/ml, injecting the lanthanum carbonate solution into the ion chromatograph, performing chromatographic analysis, and investigating method precision, wherein the result table 4 shows:
table 4: results of precision experiments
As can be seen from Table 4, the content of RSD of 6 samples with repeatability is 0.57%, the content of RSD of 6 samples with intermediate precision is 0.92%, the content of RSD of 12 samples in total is 0.84%, and the method precision is good, wherein the content of RSD of all the samples does not exceed 2.0%.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (6)
1. A method for determining the lanthanum content in a lanthanum carbonate preparation is characterized by comprising the following steps:
preparing lanthanum carbonate linear control solutions with different concentrations, respectively injecting the lanthanum carbonate linear control solutions into ion chromatography, and carrying out ion chromatography analysis, wherein the ion chromatography conditions are as follows: eluting with 5mM nitric acid solution at flow rate of 0.4ml/min, column temperature of 30 deg.C, and running time of 8 min;
calculating linear regression by taking the concentrations of different solutions as horizontal coordinates and peak areas as vertical coordinates, and establishing a standard curve to obtain a regression equation;
preparing 1000ug/ml of lanthanum carbonate sample solution, injecting the lanthanum carbonate sample solution into an ion chromatograph, carrying out ion chromatographic analysis, and calculating the lanthanum content in the sample by adopting a standard curve method.
2. The method for determining lanthanum content in lanthanum carbonate preparation according to claim 1, wherein the concentration of the lanthanum carbonate linear control solution is 400ug/ml, 600ug/ml, 800ug/ml, 1000ug/ml, 1200ug/ml respectively.
3. The method for measuring the lanthanum content in the lanthanum carbonate preparation according to claim 1, wherein the ion chromatography is performed by using a Wantong ion chromatograph-930 and a C4 guard column of 150mm by 4.0 um.
4. The method for measuring the lanthanum content in the lanthanum carbonate preparation according to claim 1, wherein the obtained standard curve is 13.001x +0.6471, and the correlation coefficient R is 0.9999.
5. The method for determining the lanthanum content in a lanthanum carbonate preparation according to claim 1, wherein the ion chromatography is performed to determine the concentration of the limiting solution at 2.8ug/ml and the concentration of the limiting solution at 0.9 ug/ml.
6. The method for measuring the lanthanum content in the lanthanum carbonate preparation according to claim 1, wherein the recovery rate of the sample solution of lanthanum carbonate is between 98% and 102%; the RSD of the recovery rate (N ═ 9) was 1.55.
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Citations (4)
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CN103037870A (en) * | 2010-05-12 | 2013-04-10 | 斯派克托姆制药公司 | Lanthanum carbonate hydroxide, lanthanum oxycarbonate and methods of their manufacture and use |
CN109001340A (en) * | 2018-09-28 | 2018-12-14 | 湖北远大天天明制药有限公司 | A kind of rapid assay methods of low concentration salt flushing liquor multicomponent content |
CN109490464A (en) * | 2019-01-24 | 2019-03-19 | 内蒙古医科大学 | A method of based on lanthanum element content in ion chromatography measurement rare earth drugs |
CN110108832A (en) * | 2019-05-29 | 2019-08-09 | 北京悦康科创医药科技股份有限公司 | A kind of measuring method of lanthanum carbonate chewable tablets dissolution curve |
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CN103037870A (en) * | 2010-05-12 | 2013-04-10 | 斯派克托姆制药公司 | Lanthanum carbonate hydroxide, lanthanum oxycarbonate and methods of their manufacture and use |
CN109001340A (en) * | 2018-09-28 | 2018-12-14 | 湖北远大天天明制药有限公司 | A kind of rapid assay methods of low concentration salt flushing liquor multicomponent content |
CN109490464A (en) * | 2019-01-24 | 2019-03-19 | 内蒙古医科大学 | A method of based on lanthanum element content in ion chromatography measurement rare earth drugs |
CN110108832A (en) * | 2019-05-29 | 2019-08-09 | 北京悦康科创医药科技股份有限公司 | A kind of measuring method of lanthanum carbonate chewable tablets dissolution curve |
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