Method for determining residual allyl amine in Sevelamer carbonate

A technology of sevelamer carbonate and allylamine, which is applied in the field of determination of residual allylamine in sevelamer carbonate, and can solve the problem that the accurate quantification of residual allylamine cannot be realized.

Inactive Publication Date: 2015-03-18
TIANJIN TAIPU PHARMA SCI & TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the limit of residual allylamine in the carbonic acid sevelamer raw material is usually set at 10ppm, which is obviously lower than the sample detection limit...

Method used

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  • Method for determining residual allyl amine in Sevelamer carbonate
  • Method for determining residual allyl amine in Sevelamer carbonate
  • Method for determining residual allyl amine in Sevelamer carbonate

Examples

Experimental program
Comparison scheme
Effect test

preparation Embodiment 1

[0075] (1) Extraction: Accurately weigh 0.5 g of sevelamer carbonate sample (batch number 130101), put it in a jar, accurately add 25 mL of distilled water, seal it tightly, extract it by ultrasonic at room temperature for 1.5 h, let it stand and cool to room temperature, 0.22 Filter through a μm filter membrane, and continue to use the filtrate for later use;

[0076] (2) Preparation of derivatization test solution: Precisely draw 10mL of the subsequent filtrate obtained in step (1) into a 50mL volumetric flask, and accurately add Na 2 CO 3 Solution 5mL, dansyl chloride stock solution 1mL, after reaction in the dark for 2h, add 2% methylamine hydrochloride solution 50μL, let it stand for 30min, dilute to the mark with distilled water, and obtain the derivatization test solution;

[0077] (3) Determination

[0078] Waters e2695 high performance liquid chromatography, Waters2475 fluorescence detector

[0079] Mobile phase: acetonitrile / water, 48 / 52(V / V)

[0080] Flow rate: ...

Embodiment 2

[0087] (1) Extraction: Accurately weigh 0.5g of sevelamer carbonate sample (batch number 130102), put it in a jar, add 25mL of distilled water precisely, seal it tightly, extract by ultrasonic at room temperature for 1h, let stand and cool to room temperature, 0.22μm Membrane filtration, continued filtrate standby;

[0088] (2) Preparation of derivatization test solution: Precisely draw 10mL of the subsequent filtrate obtained in step (1) into a 50mL volumetric flask, and accurately add Na 2 CO 3 Solution 5mL, dansyl chloride stock solution 1mL, after reaction in the dark for 2h, add 2% methylamine hydrochloride solution 50μL, let it stand for 30min, dilute to the mark with distilled water, and obtain the derivatization test solution;

[0089] (3) Determination

[0090] Waters e2695 high performance liquid chromatography, Waters2475 fluorescence detector

[0091] Mobile phase: acetonitrile / water, 50 / 50(V / V)

[0092] Flow rate: 1.0mL / min

[0093] Chromatographic column: Kr...

Embodiment 3

[0099] (1) Extraction: Accurately weigh 0.5g of sevelamer carbonate sample (batch number 130103), put it in a jar, add 25mL of distilled water precisely, seal it tightly, extract by ultrasonic at room temperature for 3h, let stand and cool to room temperature, 0.22μm Membrane filtration, continued filtrate standby;

[0100](2) Preparation of derivatization test solution: Precisely draw 10mL of the subsequent filtrate obtained in step (1) into a 50mL volumetric flask, and accurately add Na 2 CO 3 Solution 5mL, dansyl chloride stock solution 1mL, after reaction in the dark for 2h, add 2% methylamine hydrochloride solution 50μL, let it stand for 30min, dilute to the mark with distilled water, and obtain the derivatization test solution;

[0101] (3) Determination

[0102] Waters e2695 high performance liquid chromatography, Waters2475 fluorescence detector

[0103] Mobile phase: acetonitrile / water, 46 / 54(V / V)

[0104] Flow rate: 1.0mL / min

[0105] Column: Diamonsil C 18 (25...

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Abstract

The invention discloses a method for determining residual allyl amine in Sevelamer carbonate. The method includes the steps of extraction, derivatization reagent preparation and determination. The method is as below: extracting the residual allyl amine in Sevelamer carbonate by using solvents, then adding a derivatization reagent dansyl chloride in the extracting solution, adjusting the pH value with Na2CO3 solution, so that the allyl amine forms derivatization products, and determining under a fluorescence detector by a liquid chromatography method. The Na2CO3 solution has pH value of 9.5 and concentration of 0.002mg / mL; and the dansyl chloride stock solution has concentration of 0.27mg / mL. The determining method of the invention can make the allylic amine exist in a non-volatile state, stabilize the derivatization product, increase fluorescence absorption sensitivity of sample and improve the detection limit, has the advantages of accuracy, sensitivity and reliability, and provides strong scientific basis for effective control of the residual allyl amine in Sevelamer carbonate.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, and relates to a method for determining the content of impurities in drugs, more specifically to a method for determining residual allylamine in sevelamer carbonate. Background technique [0002] Sevelamer Carbonate, the chemical name is the polymer carbonate of 2-propen-1-amine and epichlorohydrin, the CAS number is 845273-93-0, and the molecular formula is (C 3 h 7 N)m.(C 3 h 5 C10)n.(CH 2 o 3 )x, the trade name is Renvela. As a drug for the treatment of hyperphosphatemia, it was developed by Genzyme of the United States. It was first launched in the United States in March 2008 and approved in the European Union in June 2009. The approved dosage forms include tablets and dry suspensions. Renvela is the next-generation product of Renagel (sevelamer hydrochloride). This product does not contain calcium and other metals. It is a non-absorbable phosphorus binder that also acts as a carb...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 吕丽娟王永福
Owner TIANJIN TAIPU PHARMA SCI & TECH DEV
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