CN101706478A - Method for testing isomer of palonosetron hydrochloride injection solution - Google Patents
Method for testing isomer of palonosetron hydrochloride injection solution Download PDFInfo
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- CN101706478A CN101706478A CN200910117598A CN200910117598A CN101706478A CN 101706478 A CN101706478 A CN 101706478A CN 200910117598 A CN200910117598 A CN 200910117598A CN 200910117598 A CN200910117598 A CN 200910117598A CN 101706478 A CN101706478 A CN 101706478A
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Abstract
The invention relates to a method for testing medicine, in particular to a method for testing isomer of palonosetron hydrochloride injection solution. The method comprises the following steps: a. preparing test solution; b. preparing mapping isomer finished solution; c. preparing mixed pretest solution, mixing the test solution and the mapping isomer finished solution with the same volume and taking the mixture as the mixed pretest solution; and d. testing the mixed pretest solution by adopting high performance liquid chromatography. The method takes isopropanol as solvent with good dissolubility and separating effect, adopts an AS-H chiral column and the mixture of normal hexane, isopropyl alcohol and diethylamine as mobile phase when testing, separates the chromatographic peak of the mapping isomer by means of completely reaching baseline, wherein the separation degree is larger than 1.5, and plays an important role in controlling the quality of the 'palonosetron hydrochloride injection solution'.
Description
Affiliated technical field
The present invention relates to a kind of detection method of medicine, particularly the method for inspection of isomeride in the palonosetron Hcl parenteral solution.
Background technology
Chipal compounds is the big difficult point in Pharmaceutical Analysis or the separation always, and the delicate variation of separation condition can directly have influence on the quality of separating resulting.The palonosetron Hcl compound has two hand-type centers, four steric isomers.Its medicine structure type is (S, S) type, (R, R) type is its enantiomter, and in addition (S, R), (R, S) type is its diastereo-isomerism, because structural similarity, especially its enantiomter (R, R) type, when utilizing liquid chromatograph to separate, because the time that the similarity of structure is successively separated is very approaching, promptly appearance time is approaching between isomeride, occur stack between each chromatographic peak easily, analyze difficulty.
Palonosetron Hcl is an ionic species, polarity is bigger, when palonosetron Hcl was detected, the sample dissolution usual way was to dissolve with methyl alcohol, though the polarity of methyl alcohol is big, but solute effect is also bad, when carrying out liquid phase analysis behind its filtrate sample introduction upper prop, the appearance time of sample is approaching, stack easily between the adjacent peak, problems such as degree of separation is bad have influenced its accuracy of detection.
Summary of the invention
The objective of the invention is to overcome existing check palonosetron Hcl and penetrate the deficiency in the isomeride method in the liquid, the method for inspection of the isomer of palonosetron hydrochloride injection solution that appearance time, peak shape and the adjacent chromatographic peak degree of separation of sample is good after a kind of easy to detect, sample introduction analysis is provided.
In order to realize this purpose, the present invention realizes in the following way: a kind of method of inspection of isomer of palonosetron hydrochloride injection solution, and this method of inspection may further comprise the steps:
Producing of a, need testing solution: get 1 part of palonosetron Hcl parenteral solution, add the 0.1-0.2 isopropyl alcohol doubly of the palonosetron Hcl parenteral solution volume of getting behind the evaporate to dryness, fully filter the dissolving back, and subsequent filtrate is need testing solution;
Producing of b, enantiomter highly finished product solution: adding the isopropyl alcohol dissolved dilution in the enantiomter highly finished product, to become concentration be about 0.05mg/mL;
Producing of c, the pre-test solution of mixing: after above-mentioned need testing solution of producing and the mixing of isopyknic enantiomter highly finished product solution, as mixing pre-test solution;
D, precision are measured the pre-test solution of above-mentioned mixing and are injected liquid chromatograph, according to high effective liquid chromatography for measuring.
According in the high effective liquid chromatography for measuring, chromatographic condition is: adopting AS-H chiral column, moving phase is the mixed solution of normal hexane, isopropyl alcohol, diethylamine, and the volume ratio of its mixing is 88: 12: 0.1 above-mentioned.
By theoretical analysis and repeatedly experiment, the present invention has following effect:
When 1) sample being handled, as solvent, dissolubility and extraction effect are good with isopropyl alcohol;
2) adopt the AS-H chiral column, normal hexane-isopropyl alcohol-diethylamine (88: 12: 0.1) is a moving phase, and the enantiomter chromatographic peak can reach baseline separation fully, and degree of separation is greater than 1.5.
3) vital role has been played in " palonosetron Hcl parenteral solution " quality control.
Description of drawings
Accompanying drawing 1 detects the chromatogram of palonosetron Hcl parenteral solution enantiomter for adopting existing method;
Accompanying drawing 2 detects the chromatogram of palonosetron Hcl parenteral solution enantiomter for adopting the inventive method.
Embodiment
1) producing of need testing solution: get palonosetron Hcl parenteral solution 100mL, place the 250mL round-bottomed flask, in 48 ℃ of decompression rotation evaporates to dryness, the accurate isopropyl alcohol 10mL that adds of sample behind the evaporate to dryness, the ultrasonic main ingredient that makes dissolves, and filters, and gets its subsequent filtrate as need testing solution;
2) producing of enantiomter highly finished product solution: in reflecting the isomeride highly finished product, add the isopropyl alcohol dissolving, be diluted to the solution that concentration is 0.05mg/mL, stand-by;
3) will go up need testing solution and isopyknic enantiomter highly finished product solution and mix, as mixing pre-test solution;
4) be that two appendix VD of Chinese Pharmacopoeia version in 2005 measure with the pre-test solution of above-mentioned mixing according to high performance liquid chromatography, during mensuration: adopt the AS-H chiral column, moving phase is adopted the mixed liquor of normal hexane, isopropyl alcohol, diethylamine, three's volume ratio is a normal hexane: isopropyl alcohol: diethylamine=88: 12: 0.1, it is 241nm that flow velocity 1.0mL/min detects wavelength, and theoretical cam curve should be not less than 2000 by the Pa Luonuosi peak.
As shown in Figure 1, 2, owing to obviously strengthen with solute effect behind the isopropyl alcohol replacement methyl alcohol, degree of separation reaches corresponding chromatographic condition regulation, and degree of separation is greater than 1.5.
The peak type chart of Fig. 1 is as follows:
Detecting device A, passage 1/241 nano wave length
The peak type chart of Fig. 2 is as follows:
Detecting device A, passage 1/241 nano wave length
Claims (2)
1. the method for inspection of an isomer of palonosetron hydrochloride injection solution, this method of inspection may further comprise the steps:
Producing of a, need testing solution: get 1 part of palonosetron Hcl parenteral solution, add the 0.1-0.2 isopropyl alcohol doubly of the palonosetron Hcl parenteral solution volume of getting behind the evaporate to dryness, fully filter the dissolving back, and subsequent filtrate is need testing solution;
Producing of b, enantiomter highly finished product solution: adding the isopropyl alcohol dissolved dilution in the enantiomter highly finished product, to become concentration be solution about 0.05mg/mL;
Producing of c, the pre-test solution of mixing: after above-mentioned need testing solution of producing and the mixing of isopyknic enantiomter highly finished product solution, as mixing pre-test solution;
D, the pre-test solution of above-mentioned mixing is adopted high effective liquid chromatography for measuring.
2. the method for inspection of isomer of palonosetron hydrochloride injection solution according to claim 1, it is characterized in that above-mentioned according in the high effective liquid chromatography for measuring, chromatographic condition is: adopting AS-H chiral column, moving phase is the mixed liquor of normal hexane, isopropyl alcohol, diethylamine, and the volume ratio of its mixing is 88: 12: 0.1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910117598A CN101706478A (en) | 2009-11-16 | 2009-11-16 | Method for testing isomer of palonosetron hydrochloride injection solution |
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| CN200910117598A CN101706478A (en) | 2009-11-16 | 2009-11-16 | Method for testing isomer of palonosetron hydrochloride injection solution |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101832981A (en) * | 2010-04-07 | 2010-09-15 | 湖北龙翔药业有限公司 | HPLC (High Performance Liquid Chromatography) method for measuring content of D-4-methylsulfonylphenyl serine ethyl ester |
| CN102495170A (en) * | 2011-11-26 | 2012-06-13 | 山东齐都药业有限公司 | Method for detecting alpha-tropine in tropisetron hydrochloride injection |
| CN104764840A (en) * | 2014-11-21 | 2015-07-08 | 重庆华邦制药有限公司 | Method for separating and detection palonosetron hydrochloride and impurity |
| CN107328880A (en) * | 2017-08-09 | 2017-11-07 | 杭州新博思生物医药有限公司 | A kind of method of reversed phase chromatography separation palonosetron hydrochloride for injection about material |
-
2009
- 2009-11-16 CN CN200910117598A patent/CN101706478A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101832981A (en) * | 2010-04-07 | 2010-09-15 | 湖北龙翔药业有限公司 | HPLC (High Performance Liquid Chromatography) method for measuring content of D-4-methylsulfonylphenyl serine ethyl ester |
| CN101832981B (en) * | 2010-04-07 | 2011-10-05 | 湖北龙翔药业有限公司 | HPLC (High Performance Liquid Chromatography) method for measuring content of D-4-methylsulfonylphenyl serine ethyl ester |
| CN102495170A (en) * | 2011-11-26 | 2012-06-13 | 山东齐都药业有限公司 | Method for detecting alpha-tropine in tropisetron hydrochloride injection |
| CN104764840A (en) * | 2014-11-21 | 2015-07-08 | 重庆华邦制药有限公司 | Method for separating and detection palonosetron hydrochloride and impurity |
| CN104764840B (en) * | 2014-11-21 | 2017-08-08 | 重庆华邦制药有限公司 | The separation of palonosetron Hcl and impurity and detection method |
| CN107328880A (en) * | 2017-08-09 | 2017-11-07 | 杭州新博思生物医药有限公司 | A kind of method of reversed phase chromatography separation palonosetron hydrochloride for injection about material |
| CN107328880B (en) * | 2017-08-09 | 2019-11-22 | 杭州新博思生物医药有限公司 | A kind of method of the reversed phase chromatography separation palonosetron hydrochloride for injection in relation to substance |
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Open date: 20100512 |