Specific rotation of this product, accurately weighed, dissolved in water and diluted per 1ml solution containing 0.2g of determination (Chinese Pharmacopoeia 2005 edition of Appendix VIE) according to the law, the specific rotation of -0.10 ° ~ +0.10 ° .
Related substances as high performance liquid chromatography (Chinese Pharmacopoeia 2005 edition two Appendix VD).
Chromatographic conditions and system suitability test with a sulfonic acid cation exchange resin as a filler, 0.005mol / L sulfuric acid solution as the mobile phase; detection wavelength of 210nm; column temperature was 37 ℃; take fumaric acid, maleic acid, DL – malic acid reference standard amount, plus the mobile phase and dilute 1ml each containing about fumarate 10μg, maleic acid 4μg, DL-malic acid solution 1mg as a system suitability solution, the precise amount of 20μl, injection liquid chromatograph, number of theoretical plates DL-malic acid peak of not less than 2000, the separation of fumaric acid and maleic acid, and DL-malic acid peaks should be required.
Determination to take this amount of goods, accurately weighed, add the mobile phase and diluted per 1ml solution containing about 1mg, as the test solution; Another reference amount of fumaric acid and maleic acid, accurately weighed with the mobile phase and dilute 1ml each containing fumaric 5μg, 2μg maleic acid solution as the reference solution. The precise amount of the two solutions of 20μl into the liquid chromatograph, record the chromatogram peak retention times to 4.5 times. For the test solution chromatogram if consistent time and fumaric acid and maleic acid peak retention peaks, the external standard method with peak area calculation, and its content should not exceed 1.0%, respectively, and 0.05%. Other single impurity peak area not more than the reference solution of maleic acid peak area of 0.5 times (0.1%); other impurities should not exceed the total amount of the reference solution of maleic acid peak area of 2.5 times (0.5%).
Clarity and color of solution of this product 5.0g, add water 25ml, fully shake to dissolve, the solution should be clear and colorless (Chinese Pharmacopoeia 2005 edition two Appendix IX AB).
Water to remove the goods, according to determination of moisture content (Chinese Pharmacopoeia 2005 edition two Appendix Ⅷ M), water containing not more than 2.0%.
Insoluble in water after taking this product 25.0g, add water 100ml dissolve, with constant weight at 100 ℃ 4 vertical melting crucible filtration, repeatedly washed with hot water filter at 100 ℃ drying to constant weight, no residue left over 0.1 %.
Easy oxides of this product 0.10g, set 100ml evaporating dish, add 25ml water and sulfuric acid solution (1 → 20) 25ml and shake to dissolve, set 20 ± 1 ℃ water bath cooling, 0.02mol / L potassium permanganate titration solution 5ml, color of the solution should not disappear within three minutes.
Chloride take this product 1.0g, according to inspection (Chinese Pharmacopoeia 2005 edition of Appendix Ⅷ A), compared with standard control solution made of sodium chloride solution 5.0ml, not thicker (0.005%).
Sulfate take this product 1.0g, according to inspection (Chinese Pharmacopoeia 2005 edition Appendix Ⅷ B), potassium sulfate solution 3.0ml comparison with the standard control solution made no thicker (0.03%).
Arsenic take this product 1.0 g, hydrochloric acid and water, 5ml 23ml, checking (Chinese Pharmacopoeia 2005 edition Appendix Ⅷ J First Act) law, shall comply with the provisions of (0.0002%).
Residue on ignition not more than 0.1% (Chinese Pharmacopoeia 2005 edition two Appendix Ⅷ N).
Heavy metals in this product 1.0g, sodium hydroxide solution 5ml and 20ml water to dissolve, according to inspection (Chinese Pharmacopoeia 2005 edition two Appendix Ⅷ H Third Law), containing heavy metals must not exceed twenty millionths.
【Assay To about 1.0g, accurately weighed, set 250ml volumetric flask, dissolved in water and diluted to the mark, shake, the precise amount of 25ml, conical flask, add 2 drops of phenolphthalein indicator solution, with sodium hydroxide (0.1mol / L) titrated to fade microscopic red and hold for 30 seconds. Each 1ml of sodium hydroxide (0.1mol / L) is equivalent to 6.704mg of C4H6O5.
[Category] pharmaceutical excipients, acidifiers, antioxidants.
[Storage] shading, sealed and stored.
