CN1948963A - Quality detecting method for likejun - Google Patents
Quality detecting method for likejun Download PDFInfo
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- CN1948963A CN1948963A CN 200610149619 CN200610149619A CN1948963A CN 1948963 A CN1948963 A CN 1948963A CN 200610149619 CN200610149619 CN 200610149619 CN 200610149619 A CN200610149619 A CN 200610149619A CN 1948963 A CN1948963 A CN 1948963A
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- acetonitrile
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- monarch
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Abstract
The invention discloses Leucogen quality detecting method. It includes the following steps: using acetonitrile or mobile phase to dissolve the Leucogen or other preparation; adding internal standard or not to form supplying testing substance solution and reference substance solution; measuring by liquid chromatogram-series connection mass spectrum method; quantifying by component peak area or component peak and internal standard peak area ratio; the liquid chromatogram condition is that the octadecylsilane chemically bonded silica is used as filer; water-acetonitrile-glacial acetic acid is as mobile phase; detecting wave is 210nm; the mass spectrum conditions are that electricity spraying ionization, positive ion detecting, 4.5kV spraying voltage, 350 degree centigrade capillary temperature, 5psi assistant atomization air (N2) air pressure, 35psi sheath air pressure, 27eV collision induced dissociation electric voltage, scanning range that m/z296-m/z132 by external standard method, Glipizide m/z 446-m/z 287 and Leucogen m/z296-m/z132 by internal standard method. The invention is advanced assaying detecting method which has the advantages of convenient operation, accuracy, sensibility, and reliability.
Description
Invention field
The present invention relates to pharmaceutical field, but disclose a kind of profit monarch's quality determining method.
Background technology
(former name: the leucogen) chemistry is by name: but 2-(α-phenyl-α-carbethoxyl group-methyl) thiazolidine-4-carboxylic acid is drug for increasing white cells to profit monarch.Structural formula is as follows:
Molecular formula: C
14H
17O
4NS molecular weight: 295.36
The leukopenia that this medicine causes owing to radiation and chemotherapy prevention, treatment, treatment alpastic anemia and thrombopenia have positive effect and radiotherapy or chemotherapeutics to use simultaneously, and clinical effectiveness is more remarkable.
Yet, but the singularity of Yin Li monarch drug in a prescription thing, what its content assaying method prolonged usefulness always is the chemistry titration method, and its limitation is arranged, the method complex operation has the chemical reagent of harmfulness greatly to operating personnel; And quality control and insolation level are lower.
But the purpose of this invention is to provide a kind of defective that has overcome content assaying method in existing profit monarch's quality determining method, and be convenient to operate, measuring method that accuracy and sensitivity, reliability all are higher than the advanced technology of former method.
Summary of the invention
But profit monarch's quality determining method of the present invention is the liquid chromatography-mass spectral detection method of contacting, but but can be used for the quality detection work of profit monarch or various profit monarch's preparations, it is characterized in that comprising following work:
(1) chromatographic condition: liquid chromatography is to be filling agent with octadecylsilane chemically bonded silica, and water-acetonitrile-glacial acetic acid is a moving phase; The detection wavelength is 210nm, external standard method; The mass spectrum condition is an electro-spray ionization, and positive ion detects, spray voltage 4.5kV, and capillary temperature: 350 ℃, assisted atomization gas (N
2) air pressure: 5psi, sheath air pressure: 35psi, collision induced dissociation voltage: 27eV;
(2) preparation of need testing solution: but the profit monarch got or its preparation thing is an amount of, precision takes by weighing, and the solution of making 100 μ g/ml with acetonitrile or moving phase is need testing solution;
(3) preparation of reference substance solution: but it is an amount of to get profit monarch reference substance, precision takes by weighing, and the solution of making 100 μ g/ml with acetonitrile or moving phase is reference substance solution.
(4) assay: respectively accurate need testing solution and the reference substance solution of drawing equal volume injected liquid chromatograph, sweep limit m/z100～300, but in the calculation sample profit monarch content to guarantee the safe and effective of product.
But profit monarch's quality determining method of the present invention, wherein the moving phase of (1) chromatographic condition is made up of water-acetonitrile-glacial acetic acid, and its best proportioning is water-acetonitrile-glacial acetic acid (56: 44: 0.3).
But profit monarch's quality determining method of the present invention, the wherein preparation of (3) reference substance solution: but precision takes by weighing profit monarch reference substance 10mg, puts in the 100ml volumetric flask, with acetonitrile or moving phase dissolving, is settled to 100ml then, is reference substance solution.
But the also available internal standard method of profit monarch's quality determining method of the present invention is measured, and internal standard compound can be Glipizide, and method is as follows:
(1) mark stock solution in: it is an amount of that precision takes by weighing Glipizide, with the acetonitrile dissolving, quantitatively is mixed with 100 μ g/ml solution, as interior mark stock solution.
(2) preparation of need testing solution: but the profit monarch got or its preparation thing is an amount of, precision takes by weighing, and with acetonitrile or moving phase dissolving, mark stock solution in accurate the adding, making Glipizide is 10 μ g/ml, and the solution of making 100 μ g/ml is need testing solution;
(3) preparation of reference substance solution: but it is an amount of to get profit monarch reference substance, precision takes by weighing, and with acetonitrile or moving phase dissolving, mark stock solution in accurate the adding, making Glipizide is 10 μ g/ml, and the solution of making 100 μ g/ml is reference substance solution.
(4) assay: accurate respectively need testing solution and the reference substance solution of drawing equal volume injected liquid chromatograph, sweep limit: Glipizide SRM (m/z446 → 287) but and profit monarch SRM (m/z296 → m/z132), but in the calculation sample profit monarch content to guarantee the safe and effective of product.
Method of the present invention is preferably come out by many tests, but but can be used for profit monarch raw material and various profit monarch's preparation.
But profit monarch's quality determining method specificity of the present invention is strong, when preparation is detected, and conventional production with the no influence of detection of auxiliary material to product.
But the sensitivity of profit monarch's quality determining method of the present invention is good, and detectability concentration is about 0.0025 μ g/ml during external standard method; Quantitatively be limited to 0.0125 μ g/ml; In 0.22-16.5 μ g/ml scope good linear relationship is arranged all, related coefficient is 0.999.Detectability concentration is about 0.0022 μ g/ml during internal standard method; Quantitatively be limited to 0.0122 μ g/ml; In 0.18-12.0 μ g/ml scope good linear relationship is arranged all, related coefficient is 0.998.
But each shows two kinds of quality determining methods of profit monarch's preparation of the present invention through 5 detection, and method precision, the testing result of eight study on the stability detections in the sample solution seven hours, three horizontal average recoveries all meets the quality testing requirement after testing.
Show that through the testing result to tens of batches of products method is better than former method in detection precision, sensitivity, and easy to operate, the solvent of use obviously descends to operating personnel's harmfulness, meets the quality testing requirement.
Claims (5)
- But 1, a kind of profit monarch's quality determining method, but but can be used for the quality detection work of profit monarch or various profit monarch's preparations, it is characterized in that comprising following work:(1) chromatographic condition: liquid chromatography is to be filling agent with octadecylsilane chemically bonded silica, and water-acetonitrile-glacial acetic acid is a moving phase, and the detection wavelength is 210nm, external standard method; The mass spectrum condition is an electro-spray ionization, and positive ion detects, and sweep limit m/z 100～300, spray voltage 4.5kV, and capillary temperature: 350 ℃, assisted atomization gas (N 2) air pressure: 5psi, sheath air pressure: 35psi, collision induced dissociation voltage: 27eV;(2) preparation of need testing solution: but the profit monarch got or its preparation thing is an amount of, precision takes by weighing, and the solution of making 100 μ g/ml with acetonitrile or moving phase is need testing solution;(3) preparation of reference substance solution: but it is an amount of to get profit monarch reference substance, precision takes by weighing, and the solution of making 100 μ g/ml with acetonitrile or moving phase is reference substance solution;(4) assay: respectively accurate need testing solution and the reference substance solution of drawing equal volume injected liquid chromatograph, measure, but in the calculation sample profit monarch content to guarantee the safe and effective of product.
- But 2, the described profit monarch's quality determining method of claim 1, wherein the moving phase of (1) chromatographic condition is made up of water-acetonitrile-glacial acetic acid, and its best proportioning is water-acetonitrile-glacial acetic acid (56: 44: 0.3).
- But 3, the described profit monarch's quality determining method of claim 1, the wherein preparation of (3) reference substance solution: but precision takes by weighing profit monarch reference substance 10mg, puts in the 100ml volumetric flask, with acetonitrile or moving phase dissolving, be settled to 100ml then, shake up, be reference substance solution.
- 4, but the also available internal standard method of the described profit monarch's quality determining method of claim 1 is measured, and internal standard compound can be Glipizide, chromatographic condition as above, other are as follows:(1) mark stock solution in: it is an amount of that precision takes by weighing Glipizide, with the acetonitrile dissolving, quantitatively is mixed with 100 μ g/ml solution, as interior mark stock solution;(2) preparation of need testing solution: but the profit monarch got or its preparation thing is an amount of, precision takes by weighing, and with acetonitrile or moving phase dissolving, mark stock solution in accurate the adding, making Glipizide is 10 μ g/ml, and the solution of making 100 μ g/ml is need testing solution;(3) preparation of reference substance solution: but it is an amount of to get profit monarch reference substance, precision takes by weighing, and with acetonitrile or moving phase dissolving, mark stock solution in accurate the adding, making Glipizide is 10 μ g/ml, and the solution of making 100 μ g/ml is reference substance solution;(4) assay: accurate respectively need testing solution and the reference substance solution of drawing equal volume injected liquid chromatograph, sweep limit: Glipizide SRM (m/z 446 → 287) but and profit monarch SRM (m/z296 → m/z132), but in the calculation sample profit monarch content to guarantee the safe and effective of product.
- But 5, profit monarch quality determining method, but but can be used for the quality testing of profit monarch raw material and various profit monarch's preparations thereof.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610149619 CN1948963A (en) | 2006-10-12 | 2006-10-12 | Quality detecting method for likejun |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610149619 CN1948963A (en) | 2006-10-12 | 2006-10-12 | Quality detecting method for likejun |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1948963A true CN1948963A (en) | 2007-04-18 |
Family
ID=38018539
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200610149619 Pending CN1948963A (en) | 2006-10-12 | 2006-10-12 | Quality detecting method for likejun |
Country Status (1)
| Country | Link |
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| CN (1) | CN1948963A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101113970B (en) * | 2007-08-28 | 2010-06-09 | 清华大学 | Mass spectra ion source without external high pressure and ionization analytical method thereof |
| CN103226142A (en) * | 2012-01-30 | 2013-07-31 | 南京长澳医药科技有限公司 | Method for detecting leucogen concentration in blood plasma |
-
2006
- 2006-10-12 CN CN 200610149619 patent/CN1948963A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101113970B (en) * | 2007-08-28 | 2010-06-09 | 清华大学 | Mass spectra ion source without external high pressure and ionization analytical method thereof |
| CN103226142A (en) * | 2012-01-30 | 2013-07-31 | 南京长澳医药科技有限公司 | Method for detecting leucogen concentration in blood plasma |
| CN103226142B (en) * | 2012-01-30 | 2016-08-10 | 上海动量医药科技有限公司 | The detection method of leucogen concentration in a kind of blood plasma |
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