CN110296948A - The remaining measuring method of palladium metal in a kind of drug - Google Patents
The remaining measuring method of palladium metal in a kind of drug Download PDFInfo
- Publication number
- CN110296948A CN110296948A CN201910736057.0A CN201910736057A CN110296948A CN 110296948 A CN110296948 A CN 110296948A CN 201910736057 A CN201910736057 A CN 201910736057A CN 110296948 A CN110296948 A CN 110296948A
- Authority
- CN
- China
- Prior art keywords
- solution
- palladium
- hydrochloric acid
- test sample
- acid
- 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
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N2001/2893—Preparing calibration standards
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The present invention provides the remaining measuring methods of palladium metal in a kind of drug, belong to heavy-metal residual analyte detection technical field.This method comprises the step of: (1) calibration curve solution is prepared；(2) standard curve is drawn；(3) test sample solution is prepared；(4) blank solution is prepared；(5) concentration mensuration；(6) calculate.Compared with prior art, the present invention is first high temperature ashing by test sample, palladium is converted into Metal Palladium or palladium oxide in organic compound, formic acid is added, palladium oxide is reduced to Metal Palladium, it is steamed near dry, aqua regia dissolution's Metal Palladium is added, the preci-sion and accuracy of palladium metal determined result of residue in drug is improved；Nitric acid is driven out of using the accurate computer heating control of hydrochloric acid, reduces influence of the nitric acid to atom spectrophotometric analysis；It is few with acid amount, reduce the pollution to environment.
Description
Technical field
The invention belongs to the remaining measurements of palladium metal in heavy-metal residual analyte detection technical field more particularly to a kind of drug
Method.
Background technique
The complete reagent of starting material, catalyst, by-product, unreacted, canister, pipe in chemical drugs synthesis process
The metal tools of road and other not acid and alkali-resistances may introduce metal impurities, and the metal residue in supplementary material can be further
It is brought into pharmaceutical preparation.Palladium is a kind of common catalyst in organic synthesis, is also commonly used in pharmaceutical production, but palladium
It is a heavy metal species, there is certain harm to human body.
Form existing for remaining palladium is uncertain in pharmaceutical production, it may be possible to Metal Palladium, palladium oxide or compound palladium, to sample
The processing of product increases difficulty.Currently, common palladium method for detecting residue is atomic absorption spectrophotometry, the side of sample treatment
Method has nitric acid-perchloric acid resolution method, the direct dissolution method of chloroazotic acid and 600 degree of ashing aqua regia dissolution's methods etc..At above-mentioned single sample
Reason method is difficult to meet requirement of experiment, moreover Metal Palladium is a kind of extraordinary catalyst, is easily turned in the treatment process of sample
Become palladium oxide.Metal Palladium is soluble in the sulfuric acid and concentrated nitric acid of chloroazotic acid and heat, but palladium oxide does not dissolve in chloroazotic acid, so using nitre
The direct dissolution method processing sample of acid-perchloric acid resolution method, chloroazotic acid is only capable of the content of Metal Palladium and palladium salt in test sample；Using
600 degree of sample ashing, add aqua regia dissolution, then hydrochloric acid are added to catch up with except method of nitric acid handles sample again, have one in 600 degree of ashing
Divide Metal Palladium transformation for palladium oxide, causes measurement result relatively low.
Summary of the invention
The purpose of the present invention is overcoming defect existing for above-mentioned existing palladium residues detecton method, providing one kind can be improved medicine
The method of the accuracy of palladium residues detecton and precision in product, this method can accurately determine the palladium content in pharmaceutical compounds,
And it is few with acid amount, reduce the pollution to environment.
In order to achieve the above object, the present invention uses following technical scheme.
The remaining measuring method of palladium metal in a kind of drug, comprising the following steps:
(1) calibration curve solution is prepared
100 μ g/ml palladium solution: precision draws 5.0ml, 1000 μ g/ml palladium standard solution in 50ml volumetric flask, with 2%
Hydrochloric acid solution is settled to graticule, mixes；
0.0 μ g/ml palladium solution: 2% hydrochloric acid solution；
0.5 μ g/ml palladium solution: precision draws 0.5ml, 100 μ g/ml palladium solution in 100ml volumetric flask, with 2% hydrochloric acid
Solution is settled to graticule, mixes；
1.0 μ g/ml palladium solution: precision draws 1.0ml, 100 μ g/ml palladium solution in 100ml volumetric flask, with 2% hydrochloric acid
Solution is settled to graticule, mixes；
2.0 μ g/ml palladium solution: precision draws 2.0ml, 100 μ g/ml palladium solution in 100ml volumetric flask, with 2% hydrochloric acid
Solution is settled to graticule, mixes；
4.0 μ g/ml palladium solution: precision draws 4.0ml, 100 μ g/ml palladium solution in 100ml volumetric flask, with 2% hydrochloric acid
Solution is settled to graticule, mixes；
(2) standard curve is drawn: using Shimadzu AA-6650 atomic absorption spectrophotometer, in wavelength: 247.6nm, electric current:
10mA, air/acetylene flame: under the conditions of 1.6~1.8:1, sample injector takes 0.0 μ g/ml, 0.5 μ g/ml palladium solution, 1.0 μ g/ respectively
Ml palladium solution, 2.0 μ g/ml palladium solution, 4.0 μ g/ml palladium solution, sequentially determining absorbance are dense then using absorbance as ordinate
Degree is abscissa, draws standard curve, obtains calibration curve formula；
(3) test sample solution is prepared
Precision weighs appropriate test sample and is added in crucible, and 1ml analytical pure sulfuric acid is added, and the carbonization on electric furnace turns
Enter and is ashed completely in 580 °~620 ° of high temperature furnace, taking out addition 5ml water, the small fire on electric furnace is steamed near dry with 1ml formic acid, after
3ml chloroazotic acid is added, small fire is steamed near dry on electric furnace, then 2ml analysis pure hydrochloric acid is added every time and catches up with nitric acid on electric furnace, repeats 3
It is secondary, it is transferred in 10ml volumetric flask, is diluted with water to scale, mix；
(4) blank solution is prepared
It takes 1ml analysis pure hydrochloric acid to be added in crucible, 1ml analytical pure sulfuric acid is added, the carbonization on electric furnace is transferred to 580 °
It is ashed completely in~620 ° of high temperature furnace, taking out addition 5ml water, the small fire on electric furnace is steamed near dry with 1ml formic acid, and 3ml is added afterwards
Chloroazotic acid, small fire is steamed near dry on electric furnace, then 2ml analysis pure hydrochloric acid is added every time and catches up with nitric acid on electric furnace, is repeated 3 times, is shifted
Into 10ml volumetric flask, it is diluted with water to scale, is mixed；
(5) concentration mensuration: under the same instrument condition of standard curve, the absorbance of test sample solution is measured, from standard
The concentration ρ of test sample solution is acquired on curve1；Under the same instrument condition of standard curve, the extinction of blank solution is measured
Degree, acquires the concentration ρ of blank solution from standard curve0；
(6) calculate: palladium metal residual quantity is in test sampleDan Wei ㎎/kg；
Wherein: ρ1- indicate that test sample solution substitutes into the concentration that calibration curve formula obtains, unit: μ g/ml；
ρ0- indicate that blank solution substitutes into the concentration that calibration curve formula obtains, unit: μ g/ml；
V-expression test sample constant volume, unit: ml；
M-expression test sample quality, unit: g；
Complete the remaining measurement of palladium metal in drug.
Above-mentioned 2% hydrochloric acid solution is to draw 20ml analysis pure hydrochloric acid, is diluted with water to the solution that 1000ml is obtained；
Above-mentioned chloroazotic acid is that 300ml is taken to analyze pure hydrochloric acid, is slowly added to 100ml thereto and analyzes pure nitric acid, stirs and mix
The solution uniformly obtained；
Above-mentioned steps (3) and (4) in the crucible that uses for glass or quartz ware.
Above-mentioned steps (3) and (4) in, the carbonization of electric furnace elder generation small fire gradually rises furnace temperature to carbonization again when carbonization.
Compared with prior art, advantageous effects of the invention:
1, test sample is first high temperature ashing, palladium is converted into Metal Palladium or palladium oxide in organic compound, and formic acid handle is added
Palladium oxide is reduced to Metal Palladium, is steamed near dry, and adds aqua regia dissolution's Metal Palladium, improves palladium metal residues detecton knot in drug
The preci-sion and accuracy of fruit；
2, since a large amount of nitric acid will affect atom spectrophotometric analysis, the present invention prepares in calibration curve solution and for sample
Using analysis pure hydrochloric acid when prepared by product, and nitric acid is driven out of using the accurate computer heating control of hydrochloric acid, reduce the concentration of nitric acid in solution,
Reduce influence of the nitric acid to atom spectrophotometric analysis.
3, glass or silica crucible are selected, avoids carrying out calcination processing to test sample using white porcelain crucible, guarantees to survey
Determine the preci-sion and accuracy of result；The carbonization of electric furnace elder generation small fire gradually rises furnace temperature to carbonization again when carbonization, prevents
Constant temperature carbonization easily causes test sample excessive to influence the preci-sion and accuracy of measurement result.
Detailed description of the invention
Fig. 1 is the remaining measuring method canonical plotting of palladium metal in drug of the invention.
Specific embodiment
Below in conjunction with the specific embodiment of the invention, technical solution of the present invention is clearly and completely described, is shown
So, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.
Embodiment
1, instrument and reagent
1) atomic absorption spectrophotometer model AA-6650, palladium lamp 247.6nm, electric current 10mA, air/acetylene flame: 1.6
~1.8:1,
2) palladium standard solution 1000ug/ml
3) sulfuric acid, nitric acid, hydrochloric acid, formic acid, perchloric acid are analytical grade reagent.
4) it 2% hydrochloric acid solution: draws 20ml and analyzes pure hydrochloric acid, be diluted with water to 1000ml；
5) chloroazotic acid: taking 300ml to analyze pure hydrochloric acid, is slowly added to 100ml thereto and analyzes pure nitric acid, stirs and mixes
It is even；
2, calibration curve solution is prepared
100 μ g/ml palladium solution: precision draws 5.0ml, 1000 μ g/ml palladium standard solution in 50ml volumetric flask, with 2%
Hydrochloric acid solution is settled to graticule, mixes；
0.0 μ g/ml palladium solution: 2% hydrochloric acid solution；
0.5 μ g/ml palladium solution: precision draws 0.5ml, 100 μ g/ml palladium solution in 100ml volumetric flask, with 2% hydrochloric acid
Solution is settled to graticule, mixes；
1.0 μ g/ml palladium solution: precision draws 1.0ml, 100 μ g/ml palladium solution in 100ml volumetric flask, with 2% hydrochloric acid
Solution is settled to graticule, mixes；
2.0 μ g/ml palladium solution: precision draws 2.0ml, 100 μ g/ml palladium solution in 100ml volumetric flask, with 2% hydrochloric acid
Solution is settled to graticule, mixes；
4.0 μ g/ml palladium solution: precision draws 4.0ml, 100 μ g/ml palladium solution in 100ml volumetric flask, with 2% hydrochloric acid
Solution is settled to graticule, mixes；
3, it draws standard curve: using Shimadzu AA-6650 atomic absorption spectrophotometer, in wavelength: 247.6nm, electric current:
10mA, air/acetylene flame: under the conditions of 1.6~1.8:1, sample injector takes 0.0 μ g/ml, 0.5 μ g/ml palladium solution, 1.0 μ g/ respectively
Ml palladium solution, 2.0 μ g/ml palladium solution, 4.0 μ g/ml palladium solution, sequentially determining absorbance are dense then using absorbance as ordinate
Degree is abscissa, draws standard curve, as shown in Figure 1,
Calibration curve formula are as follows: ABS=0.02021 ρ+0.0000275001, r=0.9999, ρ are concentration；
4, test sample solution is prepared
Precision weighs appropriate test sample and is added in crucible, and 1ml analytical pure sulfuric acid is added, and the carbonization on electric furnace turns
Enter and is ashed completely in 580 °~620 ° of high temperature furnace, taking out addition 5ml water, the small fire on electric furnace is steamed near dry with 1ml formic acid, after
3ml chloroazotic acid is added, small fire is steamed near dry on electric furnace, then 2ml analysis pure hydrochloric acid is added every time and catches up with nitric acid on electric furnace, repeats 3
It is secondary, it is transferred in 10ml volumetric flask, is diluted with water to scale, mix；
5, blank solution is prepared
It takes 1ml analysis pure hydrochloric acid to be added in crucible, 1ml analytical pure sulfuric acid is added, the carbonization on electric furnace is transferred to 580 °
It is ashed completely in~620 ° of high temperature furnace, taking out addition 5ml water, the small fire on electric furnace is steamed near dry with 1ml formic acid, and 3ml is added afterwards
Chloroazotic acid, small fire is steamed near dry on electric furnace, then 2ml analysis pure hydrochloric acid is added every time and catches up with nitric acid on electric furnace, is repeated 3 times, is shifted
Into 10ml volumetric flask, it is diluted with water to scale, is mixed；
6, concentration mensuration: under the same instrument condition of standard curve, the absorbance of test sample solution is measured, from standard
The concentration ρ of test sample solution is acquired on curve1；Under the same instrument condition of standard curve, the extinction of blank solution is measured
Degree, acquires the concentration ρ of blank solution from standard curve0；
7, calculate: palladium metal residual quantity is in test sampleDan Wei ㎎/kg；
Wherein: ρ1- indicate that test sample solution substitutes into the concentration that calibration curve formula obtains, unit: μ g/ml；
ρ0- indicate that blank solution substitutes into the concentration that calibration curve formula obtains, unit: μ g/ml；
V-expression test sample constant volume, unit: ml；
M-expression test sample quality, unit: g；
Complete the remaining measurement of palladium metal in drug.
The crucible that above-mentioned test sample uses is glass or quartz ware；If test sample calcination in porcelain crucible is handled,
The crucible of white is turned to be yellow using rear bottom, is suspected to be the compound of palladium, selects silica crucible then without this phenomenon.
The carbonization of electric furnace elder generation small fire gradually rises furnace temperature to carbonization, when test sample is carbonized not again when above-mentioned carbonization
It is overflowed from crucible.
Test example
The eltrombopag olamine for choosing three batches is test specimen.
1) the palladium content detection of eltrombopag olamine sample
Each batch sample respectively extracts 2 samples at random in three batch eltrombopag olamines, is detected by the method for embodiment, examines
The results are shown in Table 1 for survey.
The palladium content of 1 three batch eltrombopag olamine sample of table
2) precision is tested
10ug/ml palladium solution is prepared: precision draws the palladium solution of 10.0ml, 100ug/ml in 100ml volumetric flask, uses
2% hydrochloric acid solution is settled to graticule, mixes；
6 eltrombopag olamine samples are randomly selected in first batch, are numbered, and gradation precision weighs Ai Qubo by number
2ml, 10ug/ml palladium solution is added in pa 2g, is handled by the processing method for preparing test sample solution in embodiment, while into
Line blank test, and log, table 1 are the test data of precision measurement.
2 precision test data of table (concentration: the concentration of palladium in constant volume 10ml solution)
3) accuracy is tested
10ug/ml palladium solution: precision draws the palladium solution of 10.0ml, 100ug/ml in 100ml volumetric flask, with 2% salt
Acid solution is settled to graticule, mixes；
The test of 50% rate of recovery
3 eltrombopag olamine samples are randomly selected in first batch, are numbered, and gradation precision weighs Ai Qubo by number
1ml, 10ug/ml palladium solution is added in pa 2g, is handled by the processing method for preparing test sample solution in embodiment；
The test of 100% rate of recovery
It randomly selects 3 eltrombopag olamine samples again in first batch, is numbered, gradation precision weighs Chinese mugwort by number
2ml, 10ug/ml palladium solution is added in bent wave pa 2g, is handled by the processing method for preparing test sample solution in embodiment；
The test of 150% rate of recovery
It randomly selects 3 eltrombopag olamine samples again in first batch, is numbered, gradation precision weighs Chinese mugwort by number
3ml, 10ug/ml palladium solution is added in bent wave pa 2g, is handled by the processing method for preparing test sample solution in embodiment；
The palladium content for carrying out the above eltrombopag olamine sample simultaneously is tested and blank test, and log, subject to table 2
The test data of exactness measurement.
3 accuracy test data of table is following (concentration: the concentration of palladium in constant volume 10ml solution)
By above-mentioned test example, statistics indicate that, method accuracy of the invention and precision are higher, and what is determined is to have
Total palladium content in machine object, can accurately reflect palladium content in organic compound.The method is few using acid amount, reduces to ring
The pollution in border.
Based on the above content it is found that method of the invention has the valence for being applied to trace palladium content detection in all organic matters
Value.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (6)
1. the remaining measuring method of palladium metal in a kind of drug, which comprises the following steps:
(1) calibration curve solution is prepared
100 μ g/ml palladium solution: precision draws 5.0ml, 1000 μ g/ml palladium standard solution in 50ml volumetric flask, with 2% hydrochloric acid
Solution is settled to graticule, mixes；
0.0 μ g/ml palladium solution: 2% hydrochloric acid solution；
0.5 μ g/ml palladium solution: precision draws 0.5ml, 100 μ g/ml palladium solution in 100ml volumetric flask, with 2% hydrochloric acid solution
It is settled to graticule, is mixed；
1.0 μ g/ml palladium solution: precision draws 1.0ml, 100 μ g/ml palladium solution in 100ml volumetric flask, with 2% hydrochloric acid solution
It is settled to graticule, is mixed；
2.0 μ g/ml palladium solution: precision draws 2.0ml, 100 μ g/ml palladium solution in 100ml volumetric flask, with 2% hydrochloric acid solution
It is settled to graticule, is mixed；
4.0 μ g/ml palladium solution: precision draws 4.0ml, 100 μ g/ml palladium solution in 100ml volumetric flask, with 2% hydrochloric acid solution
It is settled to graticule, is mixed；
(2) standard curve is drawn: using Shimadzu AA-6650 atomic absorption spectrophotometer, in wavelength: 247.6nm, electric current:
10mA, air/acetylene flame: under the conditions of 1.6~1.8:1, sample injector takes 0.0 μ g/ml, 0.5 μ g/ml palladium solution, 1.0 μ g/ respectively
Ml palladium solution, 2.0 μ g/ml palladium solution, 4.0 μ g/ml palladium solution, sequentially determining absorbance are dense then using absorbance as ordinate
Degree is abscissa, draws standard curve, obtains calibration curve formula；
(3) test sample solution is prepared
Precision weighs appropriate test sample and is added in crucible, and 1ml analytical pure sulfuric acid is added, and the carbonization on electric furnace is transferred to
It is ashed completely in 580 °~620 ° of high temperature furnace, taking out addition 5ml water, the small fire on electric furnace is steamed near dry with 1ml formic acid, rear to add
Entering 3ml chloroazotic acid, small fire is steamed near dry on electric furnace, then 2ml analysis pure hydrochloric acid is added every time and catches up with nitric acid on electric furnace, it is repeated 3 times,
It is transferred in 10ml volumetric flask, is diluted with water to scale, mix；
(4) blank solution is prepared
Take 1ml analysis pure hydrochloric acid be added crucible in, be added 1ml analytical pure sulfuric acid, the carbonization on electric furnace, be transferred to 580 °~
It is ashed completely in 620 ° of high temperature furnace, taking out addition 5ml water, the small fire on electric furnace is steamed near dry with 1ml formic acid, rear that 3ml king is added
Water, small fire is steamed near dry on electric furnace, then 2ml analysis pure hydrochloric acid is added every time and catches up with nitric acid on electric furnace, is repeated 3 times, is transferred to
In 10ml volumetric flask, it is diluted with water to scale, is mixed；
(5) concentration mensuration: under the same instrument condition of standard curve, the absorbance of test sample solution is measured, from standard curve
On acquire the concentration ρ of test sample solution1；Under the same instrument condition of standard curve, the absorbance of blank solution is measured, from
The concentration ρ of blank solution is acquired on standard curve0；
(6) calculate: palladium metal residual quantity is in test sampleDan Wei ㎎/kg；
Wherein: ρ1- indicate that test sample solution substitutes into the concentration that calibration curve formula obtains, unit: μ g/ml；
ρ0- indicate that blank solution substitutes into the concentration that calibration curve formula obtains, unit: μ g/ml；
V-expression test sample constant volume, unit: ml；
M-expression test sample quality, unit: g；
Complete the remaining measurement of palladium metal in drug.
2. the remaining measuring method of palladium metal in a kind of drug according to claim 1, it is characterised in that: 2% hydrochloric acid
Solution is to draw 20ml analysis pure hydrochloric acid, is diluted with water to the solution that 1000ml is obtained.
3. the remaining measuring method of palladium metal in a kind of drug according to claim 1, it is characterised in that: chloroazotic acid is to take
300ml analyzes pure hydrochloric acid, is slowly added to 100ml thereto and analyzes pure nitric acid, stirs and is uniformly mixed obtained solution.
4. the remaining measuring method of palladium metal in a kind of drug according to claim 1, it is characterised in that: step (3) and (4) in
The crucible used is glass or quartz ware.
5. the remaining measuring method of palladium metal in a kind of drug according to claim 1, it is characterised in that: the step (3) and
(4) in, the carbonization of electric furnace elder generation small fire gradually rises furnace temperature to carbonization again when carbonization.
6. the remaining measuring method of palladium metal micro porpezite in non-drug organic matter in a kind of drug as described in claim 1
Belong to the application in terms of content detection.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910736057.0A CN110296948A (en) | 2019-08-09 | 2019-08-09 | The remaining measuring method of palladium metal in a kind of drug |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910736057.0A CN110296948A (en) | 2019-08-09 | 2019-08-09 | The remaining measuring method of palladium metal in a kind of drug |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110296948A true CN110296948A (en) | 2019-10-01 |
Family
ID=68032922
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910736057.0A Pending CN110296948A (en) | 2019-08-09 | 2019-08-09 | The remaining measuring method of palladium metal in a kind of drug |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110296948A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110672537A (en) * | 2019-11-12 | 2020-01-10 | 金花企业(集团)股份有限公司西安金花制药厂 | Method for determining potassium, sodium, magnesium, iron and zinc in artificial tiger bone powder |
| CN113533225A (en) * | 2020-04-13 | 2021-10-22 | 黑龙江金象生化有限责任公司 | Rapid detection method for cadmium element in tryptophan |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101196472A (en) * | 2007-05-25 | 2008-06-11 | 中国石化扬子石油化工有限公司 | Method for measuring palladium content in palladium carbon catalyzer by microwave clearing ICP method |
| CN102023154A (en) * | 2009-09-16 | 2011-04-20 | 中国石油化工集团公司 | Method for detecting the content of palladium in carbon catalyst |
| CN103575676A (en) * | 2013-11-07 | 2014-02-12 | 广州有色金属研究院 | Method for analyzing palladium in palladium-carbon catalyst |
-
2019
- 2019-08-09 CN CN201910736057.0A patent/CN110296948A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101196472A (en) * | 2007-05-25 | 2008-06-11 | 中国石化扬子石油化工有限公司 | Method for measuring palladium content in palladium carbon catalyzer by microwave clearing ICP method |
| CN102023154A (en) * | 2009-09-16 | 2011-04-20 | 中国石油化工集团公司 | Method for detecting the content of palladium in carbon catalyst |
| CN103575676A (en) * | 2013-11-07 | 2014-02-12 | 广州有色金属研究院 | Method for analyzing palladium in palladium-carbon catalyst |
Non-Patent Citations (4)
| Title |
|---|
| 崔增团等: "《测土配方施肥指南》", 31 December 2014, 甘肃科学技术出版社 * |
| 庄伊美主编: "《柑桔营养与施肥》", 31 December 1994, 中国农业出版社 * |
| 韩继永等: "火焰原子吸收分光光度法测定替加环素中的痕量钯", 《华西药学杂志》 * |
| 魏小娟等: "电感耦合等离子体原子发射光谱法测定废钯炭催化剂中钯", 《冶金分析》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110672537A (en) * | 2019-11-12 | 2020-01-10 | 金花企业(集团)股份有限公司西安金花制药厂 | Method for determining potassium, sodium, magnesium, iron and zinc in artificial tiger bone powder |
| CN113533225A (en) * | 2020-04-13 | 2021-10-22 | 黑龙江金象生化有限责任公司 | Rapid detection method for cadmium element in tryptophan |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104215651B (en) | Method for measuring content of sulfur in coal by utilizing energy chromatic dispersion X-ray fluorescence analysis | |
| CN103412034A (en) | Measuring method for quickly measuring contents of heavy metals in tobacco by using microwave digestion/ICP-MS method | |
| CN107976481B (en) | Method for detecting scandium content in traditional Chinese medicinal materials | |
| CN109406690B (en) | Method for detecting related substances in chloral hydrate | |
| CN110296948A (en) | The remaining measuring method of palladium metal in a kind of drug | |
| CN109100309A (en) | Dispersive liquid-liquid microextraction-Android mobile phone colorimetric estimation micro calcium ion method | |
| CN109163958A (en) | A kind of Methods of Soil Digestion and a kind of detection method for measuring various heavy in soil simultaneously | |
| CN105758830A (en) | Method for measuring content of total arsenic by digesting marine product in steps through microwave humidifying method | |
| CN104215627A (en) | Method for microwave digestion-inductively coupled plasma mass spectrometer (ICP-MS) determination of metal ions such as lead, arsenic, cadmium and chromium in cigarette case | |
| CN109738419B (en) | Method for measuring boron content in aluminum-based boron carbide material | |
| CN105651722B (en) | A kind of public English ultramarine mixture method of quality control based on ultraviolet fingerprint | |
| CN108593606B (en) | Method for testing germanium content in coal by utilizing atomic fluorescence spectroscopy | |
| CN105606435A (en) | Pretreatment method for measuring content of mercury in soil and detection method using same | |
| CN110220887B (en) | Method for measuring lead, zinc, tin and nickel in waste circuit board stripping material resin powder | |
| CN103115881B (en) | Evaluate and reduce the method for the uncertainty numerical value of potassium in iron ore | |
| CN110044876A (en) | A kind of full Boron nitrogen rings method in low-alloy steel | |
| CN110389166A (en) | The rapid detection method of heavy metal limit in a kind of food additives | |
| CN110146490A (en) | A method of with micro ruthenium element in ICP-OES measurement drug | |
| Völlkopf et al. | Determination of cadmium, copper, manganese and rubidium in plastic materials by graphite furnace atomic absorption spectrometry using solid sampling | |
| CN114414539B (en) | Method for measuring content of bismuth and antimony elements in roasted molybdenum concentrate | |
| Zhang et al. | Determination of Pb in geological materials by heat extraction slurry sampling ET-AAS | |
| CN105987965A (en) | Method for determining various types of abuse drugs in human whole blood | |
| CN103207170A (en) | Method for analyzing and determining arsenic form in liquid food seasoning | |
| CN101435777B (en) | Method for testing amino silicon oil content in chitosan fiber | |
| CN110161028A (en) | Utilize the method for the perchlorate in DLLME and scanner digital image analysis measurement food |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20191001 |
|
| RJ01 | Rejection of invention patent application after publication |