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Wysłany: Śro 10:22, 16 Mar 2011
Temat postu: herve leger skirts acm jit dpk buy
More nail Ma Min (U.S. available) syrup Improved HPLC Determination
Separation is not ideal, but a long retention time of dextromethorphan hydrobromide injection in several follow-up after the injection of disruption. To solve the above problem, the author improved this method can effectively control the quality of the preparation. 1. Instrument and reagent Shimadzu LC-lOAvp HPLC,
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, LC-10ATvp pump,
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, SPD a 10Avp UV detector. Dextromethorphan reference substance, reference substance Guaifenesin, phenylpropanolamine hydrochloride reference standard and reference standard chlorpheniramine maleate by Beijing Pharmaceutical Co., Ltd. to provide Bao Sheng Delai, purity was 100. 6%, 99I8%, 100.3% and 100.5%. Acetonitrile for chromatography pure, high water, phosphoric acid is superior pure, triethylamine were of analytical grade. More nail Ma Min (U.S. available) syrup Shengde Lai Bao Pharmaceutical Co., Ltd. from Beijing to provide (batch number: 04060206,04080206). 2. Chromatographic conditions and system suitability testing system 1 (Determination of Guaifenesin, phenylpropanolamine hydrochloride and chlorpheniramine maleate) column: CAPCELLPAKCl8 column (150mmx4.6mm, 5m),
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, mobile phase: buffer (containing 1 % =-- ethylamine and 1.1% phosphoric acid solution, pH value is adjusted with triethylamine 2.10 ~ 0.05) of a acetonitrile gradient elution program is 0.0-16.5 minutes acetonitrile 13%, to 16.6 minutes,
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, increasing to 35% acetonitrile, maintaining to 25.0 minutes to 25.1 minutes, returned to 13% acetonitrile, maintaining to 40.0 minutes. Flow rate of 1. Oml / min, detection wavelength 220nm, column temperature 30 ℃, and the injection volume 20l. In the chromatographic conditions, the test record survived glyceryl ether,
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, phenylpropanolamine hydrochloride and chlorpheniramine maleate in the number of theoretical plates were 10648,6924,9663; phenylpropanolamine hydrochloride and chlorpheniramine maleate peak separation between 20.5; Chlorpheniramine Maleate and Guaifenesin separation between the peak of 10.2. Preparation does not affect other components of the determination of the three components. System 2 (Determination of dextromethorphan hydrobromide) column: CAPCELLPAKCl8 column (150mmx4.6mm, 5txm), mobile phase: buffer (containing 1% triethylamine and 1.1% phosphoric acid solution, adjusted with triethylamine pH = 2.10 ~ 0.05) a acetonitrile (65:35), flow rate 1.0ml/min, detection wavelength 220nm, column temperature 30 ℃, and the injection volume 2Oral. In the chromatographic conditions, dextromethorphan hydrobromide measured theoretical plate number was 7078; dextromethorphan and the separation between adjacent peaks is greater than 3-8. Preparation does not affect the other components in the determination of composition. 3. Precision of chromatographic system 1 according to the conditions of the same sample solution (batch 04060206) repeat sample 5 times, Guaifenesin peak area RSD was 0.10%, salt content of the sample determination results Schedule (labeled amount %. n = 2) phenylpropanolamine acid peak area RSD was 0.52%, chlorpheniramine maleate peak area RSD of 0.49%. 2 according to the conditions of chromatography system of the same sample solution (batch 04060206) repeat sample 5 times, dextromethorphan hydrobromide peak area RSD was 0.15%. 4. Sample assay methods using national standards 【1】 sample preparation, and after 0.45txm microporous membrane filtration, measured by the improved method to measure the results of the Annex. 5. 5.1 This method increases the discussion of triethylamine and phosphoric acid concentration, and adjust the buffer pH. Thus, by controlling the flow of the first phase of the secondary chemical equilibrium to improve selectivity, to achieve better separation; wrap up the second dose increased the amount of triethylamine, can effectively suppress trailing slightly alkaline substances; Third Regulator pH value, can better protect the column (before adjusting pH value is only about 1.85.) 5.2 Application of the chromatographic system 1, gradient elution can be retained when a Secretary of dextromethorphan eluted in a relatively short period of time, will not cause the front left peak Diego dextromethorphan hydrobromide analytes added to the back of the peak, thus ensuring the accuracy of the determination results. 5.3 pairs of column temperature requirements are not necessary to room temperature. 5.4 The sample solution through the microporous membrane filtration 0.45txm, you can remove most of the coloring agent, beneficial for the protection of the column.
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