Method for determination of optical isomers in palonosetron hydrochloride composition

A technology of palonosetron and optical isomers, which is applied in the field of medicine and can solve the problems that the accurate determination of impurity content has an influence, and the diastereomers cannot be detected at the same time.

Active Publication Date: 2012-08-15
JIANGSU AOSAIKANG PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The detection method in the prior art, the chromatographic conditions in the Chinese patent ZL200710074410.0 (notification number CN101303331B) can only control the enantiomer, but cannot detect the other two diastereoisomers at the same time, need to use Two different chromatographic conditions were determined separately
When one of the diastereomers is determined, the other diastereomer will overlap with the main peak, which will affect the accurate determination of the impurity content

Method used

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  • Method for determination of optical isomers in palonosetron hydrochloride composition
  • Method for determination of optical isomers in palonosetron hydrochloride composition
  • Method for determination of optical isomers in palonosetron hydrochloride composition

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Instrument: Shimadzu LC-10AT high performance liquid chromatography system, including LC-10AT pump, SPD-10A ultraviolet detector and HW chromatography workstation.

[0020] Chromatographic column: chiral chromatographic column Chiralpak ADH column (250mm×4.6mm, 5μm).

[0021] Mobile phase: n-hexane-absolute ethanol-diethylamine (93:7:0.2)

[0022] Detection wavelength: 240nm

[0023] Flow rate: 0.6ml / min

[0024] Column temperature: 20°C

[0025] Reference substance solution: Accurately weigh an appropriate amount of R, R-type palonosetron reference substance, S, R-type palonosetron reference substance and R, S-type palonosetron reference substance, and add mobile phase to quantitatively dilute Prepare a mixed solution containing about 0.5 μg in each 1 ml as a reference solution.

[0026] Need testing solution: take 10 palonosetron hydrochloride compositions, put them in an evaporating dish, concentrate in a water bath to about 5ml, let it cool, add 40ml of ethanol,...

Embodiment 2

[0028] Example 2 Determination of Palonosetron Hydrochloride Composition Preparation Method

[0029] prescription:

[0030] Palonosetron Hydrochloride 0.28g

[0031] Mannitol 207.5g

[0032] Sodium edetate 0.5g

[0033] Citric acid 25g

[0034] Water for injection 5000ml

[0035] Made 1000 pieces

[0036] Weigh the prescribed amount of mannitol, edetate sodium and citric acid, add to 96% water for injection, stir to dissolve, add 0.1mol / L sodium hydroxide solution, adjust the pH value to about 5.0 (4.5-5.5), Add 0.1% activated carbon for needles, stir at 80°C for 30 minutes, decarbonize with a titanium alloy rod while it is hot, then add the prescribed amount of palonosetron hydrochloride, stir to dissolve, make up to the full amount with water for injection, and then inject 0.22μm Filter through a microporous membrane until clear, measure the intermediate content and pH value, and fill it in ampoules with 5ml per bottle, seal it, sterilize it at 121°C for 15 minutes...

Embodiment 3

[0038] According to Example 2, three batches of palonosetron hydrochloride composition samples were prepared and the content of palonosetron hydrochloride isomers in each batch of compositions was detected. The specific results are shown in Table 1.

[0039] Table 1 Inspection results of palonosetron hydrochloride isomers in the palonosetron hydrochloride composition

[0040] Batch number RR isomer RS type isomer SR isomer 100501 not detected not detected not detected 100502 not detected not detected not detected 100503 not detected not detected not detected

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Abstract

The invention provides a method for detecting palonosetron hydrochloride isomers in a palonosetron hydrochloride composition. The method adopts a chiral chromatographic column with amylose tris(3,5-dimethylphenylcarbamate) as filler; n-hexane/absolute ethyl alcohol /diethylamine as a mobile phase; and a detection wavelength of 240nm. The method comprises the following steps of preparing 0.5mug/ml of a solution containing palonosetron hydrochloride isomers with the mobile phase as a reference solution, performing determination and recording the spectra. The method provided by the invention can effectively separate three optical isomers of palonosetron hydrochloride under the same chromatographic conditions, and the separation degree between palonosetron hydrochloride and each of the isomers of palonosetron hydrochloride can be up to 1.5 to 2.0, which is in line with the requirements of Chinese Pharmacopoeia. The method provided by the invention can also be used for quantitative determination of palonosetron hydrochloride isomers.

Description

technical field [0001] The invention belongs to the field of medicine, and more specifically relates to a method for detecting isomers of palonosetron hydrochloride in a palonosetron hydrochloride composition. Background technique [0002] The chemical structural formula of Palonosetron Hydrochloride is: [0003] [0004] The chemical name is: 2-[1-azabicyclo(2.2.2)oct-3S-yl]-2,3,3aS,4,5,6-hexahydro-1H-benzo[de]isoquinoline- 1-Keto hydrochloride. [0005] Palonosetron hydrochloride is a 5-hydroxytryptamine receptor antagonist developed by Helsinn Healthine Company in Switzerland. It is a white or off-white powder. This product is very soluble in 0.1mol / L hydrochloric acid solution and water, dissolved in methanol, Very slightly soluble in ethanol, almost insoluble in 0.1mol / L sodium hydroxide solution. Its injection was launched in the United States in September 2003 under the trade name Aloxi ? ;Clinically, it is mainly used to treat vomiting reactions duri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/36
Inventor 任凤杨奇珍
Owner JIANGSU AOSAIKANG PHARMA CO LTD
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