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The existing literature on fingerprint chromatography at home and abroad and the quality control of biochemical injection with multiple components were reviewed in this article.Combined with the laboratory research, It is proposed that the strategy for HPLC specific chromatography of biochemical injection with multiple components in order to provide the basis for effectively promoting the establishment and development of HPLC specific chromatography of biochemical injection with multiple components.
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Objective To investigate the influencing factors and improve potency methods of chymosin, to verify the stability and applicability of the national standard of chymosin.Methods The effects of different formula milk powder substrate and enzyme concentration on the determination of the activity of chymosin were studied.3 ×3 dose-response parallel line method was established.The results were compared with the different methods of absolute and relative methods.Results The different formula milk powder had a significant effect on the determination of the absolute potency of the activity of chymosin.The concentration of the enzyme was a power function relationship with the milk clotting time.Compared with the absolute potency, reproducibility of the relative potency of the results was better in different laboratories.The suitable doses in 3 ×3 dose-response parallel line method were 0.35,0.44,0.55U/mL.The confidence limit rate was less than 5%.The potency of the national standard of chymosin (140712-201302) was not significantly different between 2013 and 2015.In a certain dose range, the dose-response of the national standard of chimosin and gastropylor complex or lamb'tripe extract was linear, and the two lines were parallel.Conclusion A lot of factors can affect on the potency of chymosin.Relative potency is determinate by reference standard which can eliminate the influence of different substrates, different operators and endpoint judgment on the determination in order to make results have comparability between laboratories.The test design of 3 ×3 dose-response parallel line can control the test deviation better than the single point determination.The stability of the national standard of chymosin(140712-201302) is good, and is suitable for the potency of chymosin of the products of gastropylor complex and the extract of the lamb.
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Objective To improve the related substances analysis method of cobamamide.And to further research light degradation characteristics of cobamamide.Methods Determined the related substances of solid and aqueous solution of cobamamide after light degradation by high performance liquid chromatography(HPLC) conditions,which is Merck Hibar C18 column (4.6 mm ×250 mm, 5μm), 0.05 mol/L KH2PO4 solution:acetonitrile (90:10) -80% acetonitrile as mobile by gradient elution and detection wavelength 260 nm.And compared their light stability.The main three kinds of light degradation impurities were determinate from LC-MS.Results Gradient elution made the light degradation impurities separate better.The results of precision and reproducibility tests increased to RSD =0.2% (n=6) and RSD =8% (n=5) from RSD =3.8% (n =6) and RSD=38%(n=5). Cobamamide solution was very sensitive to light, the preparation should be strict dark operation.Two of the light degradation impurities were adenosine and hydroxycobalamin, with the relative response factor 2.5 and 0.7.Conclusion New method is specific, durable and reproducible, which can be used for quality control of cobamamide.
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Objective To analyze peroxide value and anisidine value of ethyl polyenoate soft capsules and imported drugs and evaluate the oxidative stability.Methods The analysis was carried out on a TSK gel ODS-100 V(250 mm ×4.6 mm,5μm)with methanol-water(98:2,V/V)as the mobile phase to determine the structure of the vitamin E as antioxidant.The influence on the antioxidation effect of tocopherol acetate andα-tocopherol as excipient in omega-3 polyunsaturated fatty acid ethyl ester drugs was evaluated.Results The structure of vitamin E as antioxidant in domestic drugs was acetate, while vitamin E as excipient in foreign drugs had the structure of α-tocopherol monomer.As antioxidant, the antioxidation effect of tocopherol acetate was better thanα-tocopherol.The structure of vitamin E had a direct impact on the antioxidation effect of omega-3 polyunsaturated fatty acid ethyl ester drugs.Conclusion The studies provide the basis for evaluate rationality of antioxidant in ethyl polyenoate soft capsules scientifically, which has positive significance for controlling the quality of the drug effectively.
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Objective To establish the dissolution curves test method of Ribavirin capsules, and investigate dissolution behavior of domestic Ribavirin capsules.To provide experimental basis for generic drugs quality consistency evaluation.Methods According to the first dissolution method (basket method)stated in appendix Ⅹof Chinese Pharmacopeia(2010 edition),the rotation speed was 50 r/min with dissolution medium volume of 900 mL.The dissolution profiles of Ribavirin capsules in four different mediums( pH 1.2 hydrochloric acid solution,pH 4.5 acetic buffer,pH 6.8 phosphate buffer and water) were determined by HPLC.The determination was performed on C18 column with mobile phase consisted of 4 g/L sodium dihydrogen phosphate solution(pH adjusted to 5.0 ±0.05 using 5% sodium hydroxide solution)-acetonitrile(98:2)at the flow rate of 1.0 mL/min.The detection wavelength was 225 nm,and sample size was 10μL.Results The linear range of ribavirin was 2.5-200μg/mL(r=1).RSD of precision and stability tests were lower than 0.5%.The average recoveries were 101.3%, 100.7%, 100.2%, 100.4% in four mediums.Dissolution behavior of capsules can be more consistent and rapid dissolution in pH4.5 and pH6.8 mediums.But they were quite different in pH1.2 and water mediums, and some of their average dissolution at 15 min could not reach 85%.Conclusion This method is accurate and reliable.There is a difference between domestic Ribavirin capsules dissolution behavior, and the formulation processes have room for improvement.
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Objective To establish the chromogenic substrate method to determine the activity of cytochrome C.Methods Used TMB as the chromogenic substrate, reacted at 37 ℃ for 15 min, generated the yellow products, and detected the absorbance at 450 nm.The experimental design method is the 4 ×4 parallel line quantitative analysis.ResuIts The activities of cytochrome C injection samples have been determined.The linear regression equation was Y=0.9875 X -1.0221,R2 =0.9996.The accuracy and repeatability were 1.1 % and 3.6 %.ConcIusion The chromogenic substrate method was simple operation, sensitive and can be used to determine the activity of cytochrome C.
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Therapeutic oligonucleotides have been one of the hottest areas in R&D of drugs in recent years.The research of analysis method has been widely carried out.Ion-pairing reverse liquid chromatography is the most commonly used method for good resolution and easy docking with MS.A review is presented here on the progress of oligonucleotides analysis with ion-pairing reverse liquid chromatography.The column, mobile phase, MS detection, mechanism of analysis will be discussed.
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Objective To establish a method to quantify the residual cross-linker vinyl sulfone and its hydration product 1 ,4-Thioxane-1 ,1-Dioxide.Methods The polysaccharide was precipitated by ethanol,however vinyl sulfone and its hydration product were soluble,and can be analyzed by direct injection.The analysis was carried on Agilent DB-wax capillary column (30m ×0.53 mm,1.0 μm).The flame ionization detector (FID)and flame photometric detector (FPD)were used to detect samples and the efficiency were compared. Results The linear range of vinyl sulfone and its hydration product were separately 0.5 ~20μg/mL and 2~100μg/mL detected by FID.The Limit of Quantity (LOQ)were 0.8μg/mL and 2.3μg/mL, respctively.The Limit of Detection (LOD)were 2.6μg/mLand 7.6μg/mL,respectively,and the average recoveries (n=9)of them were 104.3%and 92.4%,respectively.Conclusion FID could meet the needs of the test,and this method is simple and accurate with high sensitivity and good repeatability,which can be used for quality control of trace vinyl sulfone and its hydration products 1 ,4-Thioxane-1 ,1-Dioxide in cross-linked sodium hyaluronate injection.
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Purpose Semi-macro-chromogenic substrate methods have been adopted by British Pharmacopoeia to determine the anti-F Ⅹ a activity and anti-F Ⅱ a activity of low molecular weight heparin. Based on the above methods, the micro-chromogenic substrate methods were established to determine the anti-F Ⅹ a and anti-F Ⅱ a activity of heparins. Methods After the adjustment of the concentration of reagents and the whole volume of the test, 96-well microplates and the microplate spectrophotometer have been used to determine the absorbance. Results Six samples of heparin's potencies of anti-F Ⅹ a and anti-F Ⅱ a have been determined. The test results show that the errors of the tests are small and the repeatability is good. Conclusion Micro-chromogenic method can be used to determine the activity of anti-F Ⅹ a and anti-F Ⅱ a of heparins. This method improved the efficiency of the test and decreased the cost of the test. Mow the chromogenic substrate methods are being considered as the pharmacopoeia methods to substitute the anticoagulant methods.