Method for detecting basic lanthanum carbonate impurities in lanthanum carbonate raw material or preparation thereof in solid state

A technology of lanthanum carbonate and lanthanum carbonate, which is applied in the field of analytical chemistry and can solve problems such as the inability to analyze and detect lanthanum carbonate degradation impurity lanthanum carbonate

Inactive Publication Date: 2019-12-17
北京华睿鼎信科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The technical problem to be solved in the present invention is to overcome the technical difficulty that conventional techniques cannot analyze and detect lanthanum carbonate or its prepara

Method used

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  • Method for detecting basic lanthanum carbonate impurities in lanthanum carbonate raw material or preparation thereof in solid state
  • Method for detecting basic lanthanum carbonate impurities in lanthanum carbonate raw material or preparation thereof in solid state
  • Method for detecting basic lanthanum carbonate impurities in lanthanum carbonate raw material or preparation thereof in solid state

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0086] specificity test

[0087] Instrument test conditions: Rigaku D / max-rA X-ray diffractometer, using Cu Kα target, tube pressure and tube flow are 40KV and 100mA respectively; divergence slit and anti-scatter slit are 1°, receiving slit is 0.30mm , the detector is a sodium iodide scintillation counter, θ-2θ linkage continuous scanning, the scanning rate is 2° / min (0.02° step width), and the scanning range is 9-40°.

[0088] Test procedure: 1) lanthanum carbonate sub-carbonate I, 2) lanthanum subcarbonate II, 3) lanthanum carbonate raw material (excluding sub-lanthanum carbonate I and II), 4) lanthanum carbonate chewable tablet fine powder, 5) corundum , 6) lanthanum carbonate + lanthanum carbonate sub I + lanthanum sub carbonate II + corundum mixture, 7) lanthanum carbonate chewable tablet fine powder + lanthanum carbonate sub I + lanthanum sub carbonate II + corundum mixture, carry out PXRD scanning after sample preparation respectively, record Spectrum, see the results ...

Embodiment 2

[0096] Linearity and Range Tests

[0097] A. the lanthanum carbonate sample that does not contain basic lanthanum carbonate I and II is fully pulverized to obtain the lanthanum carbonate sample fine powder;

[0098] b. add different quality lanthanum carbonate I and lanthanum carbonate II respectively in the lanthanum carbonate that does not contain lanthanum carbonate I and II,

[0099] Standard curve sample 1: lanthanum carbonate contains 8.16% lanthanum carbonate sub-II and 9.12% sub-lanthanum carbonate II;

[0100] Standard curve sample 2: Lanthanum carbonate contains 6.8% lanthanum carbonate sub-I and 7.6% sub-lanthanum carbonate II;

[0101] Standard curve sample 3: lanthanum carbonate contains 5.44% lanthanum carbonate sub-I and 6.08% lanthanum sub-carbonate II;

[0102] Standard curve sample 4: lanthanum carbonate contains 3.4% lanthanum carbonate sub-I and 3.8% lanthanum sub-carbonate II;

[0103] Standard curve sample 5: Lanthanum carbonate contains 1.36% of lanth...

Embodiment 3

[0118] repeatability test

[0119] When investigating repeatability, prepare 6 parts of samples in parallel by the method of standard curve sample 2, after scanning PXRD respectively, measurement result is substituted in embodiment 2 standard curve equations, calculates the recovery amount of lanthanum subcarbonate I and lanthanum subcarbonate II, Investigate the RSD of the calculation results among the 6 samples, the results are as follows:

[0120]

[0121]

[0122] Conclusion: The test results show that the repeatability of this method is good.

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Abstract

The invention provides a method for detecting basic lanthanum carbonate impurities in a lanthanum carbonate raw material or a preparation thereof in a solid state. The method comprises the following steps: fully grinding lanthanum carbonate or a preparation thereof, adding different amounts of basic lanthanum carbonate, fully and uniformly mixing the mixture with corundum according to a certain ratio to prepare a series of standard curve samples, scanning each standard curve sample by using a powder X-ray diffraction method, and drawing a standard curve to obtain a linear equation; fully and uniformly mixing to-be-detected lanthanum carbonate or a preparation thereof with corundum according to a certain ratio to prepare a test sample; carrying out measurement based on the same way, substituting a ratio of the diffraction intensities of the characteristic peaks of the basic lanthanum carbonate and corundum in the test sample into a linear equation to calculate the content of basic lanthanum carbonate in the sample. The method can be used for analyzing and detecting basic lanthanum carbonate impurities in lanthanum carbonate or lanthanum carbonate preparations. The method has advantages of simple operation, wide linear range, good linear relation, high precision, high accuracy, high durability and high detection sensitivity.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, in particular to a method for analyzing and detecting basic lanthanum carbonate impurities using powder X-ray diffraction (PXRD), more specifically, to a method for analyzing and detecting basic lanthanum carbonate impurities in lanthanum carbonate or its preparations. Lanthanum carbonate method. [0002] technical background [0003] Hyperphosphatemia is a common complication in patients with chronic kidney disease (CKD), especially end-stage renal disease (ESRD), and can be found in 80% of dialysis patients. The current treatment measures for hyperphosphatemia mainly limit phosphorus intake, adequate dialysis, use of phosphorus binders, and parathyroidectomy plus autologous transplantation when necessary. [0004] Traditional phosphorus binders are mainly aluminum-containing and calcium-containing phosphorus binders. The traditional aluminum salts of phosphorus binders can cause toxic side e...

Claims

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Application Information

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IPC IPC(8): G01N23/2005G01N23/20
CPCG01N23/20G01N23/2005G01N2223/0568G01N2223/1016G01N2223/652
Inventor 安明常珍况斌祝江业张婵娟杨清燕
Owner 北京华睿鼎信科技有限公司
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