Establishment of an in vitro fluorescence spectrophotometry based on end-product malondialdehyde for evaluating scavenging ability on hydroxyl radicals / 中国药理学通报

Aim To establish an in vitro fluorescence spectrophotometry based on the end-product malondialdehyde(MDA)for evaluating hydroxyl radical-scavenging ability, and compare the advantages and disadvantages of fluorescence and visible methods.Methods The reaction time, temperature, and the concentration of key reactant deoxyribose were investigated and optimized respectively.Under different solvent conditions, sensitivity and the measurement window of two methods were compared.The hydroxyl radical scavenging ability of tanshinone I was determined by these two methods.Results The optimal temperature and time was 37 °C and 60 min, and the concentration of deoxyribose was 2.8 mmol·L-1.The limit of detection for the fluorescence method(4.49 nmol·L-1)was much lower than that of the visible spectrophotometry(39.15 nmol·L-1).The ratio of model/control(the measurement window)of the fluorescence method was much larger than that of visible spectrophotometry in both the aqueous system and the organic system(containing DMSO).Within the concentrations of 62.5 mg·L-1-1 000 mg·L-1, tanshinone I showed scavenging ability on hydroxyl radicals in a concentration-dependent manner using the fluorescence method, but the visible method could not.Conclusions In contrast to visible method, fluorescence method has the advantages of higher sensitivity and stronger anti-interference ability to the color of test substance and the specificity of solvents.By virtue of large measurement window, it can be applied to evaluating the effect of fat-soluble test substances.

Analytical Method Development And Its Validation For Estimation Of Chlorhexidine Gluconate

In the present work, Independent method was developed for estimation of Chlorhexidine Gluconate, Metronidazole benzoate,Lignocaine Hydrochloride, and Salicylic Acid in bulk and dosage form by UV-Visible Spectrophotometry. In this method the determination ofmaximum absorbance (λmax) of the drugs were found to be 259 nm, 285.8 nm, 263 nm and 304 nm. The validation parameters were studiedaccording to ICH guidelines. On the basis of % agreement criteria, therefore Average % agreement found to be 100.05 at 259 nm, 99.32 at285.8 nm, 100.001 at 304 nm and 99.70 at 263 nm. Specificity study shows the good agreement with results, indicating that excipients did notinterfere with the analyte. Repeatability study showed a % R.S.D of 0.2486 at 259 nm, 0.2605 at 285.8 nm, 0.403174 at 304 nm and 0.880817at 263 nm for Chlorhexidine Gluconate, Metronidazole benzoate, Lignocaine Hydrochloride, and Salicylic Acid. Thus it is concluded that theanalytical technique has a good repeatability precision as R.S.D are less than 5.3% (Specified) and less than 2% (desired). So it can be said thatthe proposed method is precise. Intraday study were showed a % R.S.D of 1.246918, 0.984763, 0.775939 and 1.022045 respectively forChlorhexidine Gluconate, Metronidazole benzoate, Lignocaine Hydrochloride, and Salicylic Acid. So it can be said that the proposed method isprecise. Interday study were showed a % R.S.D of 1.358486, 0.829325, 1.273356 and 0.968196 respectively for Chlorhexidine Gluconate,Metronidazole benzoate, Lignocaine Hydrochloride, and Salicylic Acid. So it can be said that the proposed method is precise. Limit of detectionwere found to be 0.097, 0.117, 0.010 and 0.074 g/ml at 259, 285.8, 304and 263 nm. Limit of quantification were found to be 0.29, 0.35, 0.030and 0.418 g/ml at 259, 285.5 304, and 263nm. The accuracy of the methods was proved by performing recovery studies in availableformulations. Since the % recovery 98.07 to 101.28 at 259 nm, 98.29 to 101.02 at 285.8 nm, 99.99 to 101.25 at 304nm and 99.10 to 101.78 at263nm are within the desirable confidence interval of 98-102%. So it can be said that the proposed method is accurate. The percent meanrecovery is 98.46, 101.42 (1:3), 98.20 and 99.78% of labeled amount, which is within specified limits of 98-102%. It can be said that proposedmethod can satisfactory be applied for analysis of Chlorhexidine Gluconate, Metronidazole benzoate, Lignocaine Hydrochloride, and SalicylicAcid in dosage form. The developed method is precise, accurate and do not suffer from any interference due to common excipients. It isevident from this study that the developed method is simple, sensitive, specific, precise and accurate and economic. Hence it can be employedfor routine analysis in quality control laboratories.

Study on Quality Standard of Chailing Hugan Granules / 中国药房

OBJECTIVE:To establish the quality standard of Chailing hugan granules. METHODS:TLC was used for qualitative identification of Radix bupleuri,Atractylodes macrocephala and Glycyrrhiza uralensis. The content of total flavonoids (by rutin) in preparation was determined by UV-visible spectrophotometry. The moisture, dissolubility and granularity of preparation were determined. RESULTS:TLC spots of R. bupleuri ,A. macrocephala and G. uralensis were clear and well-separated without interference from negative control. The linear range of rutin was 0.050-0.300 mg/mL(r＝0.999 8). RSDs of precision, stability and reproducibility tests were all lower than 2%. The recoveries were 97.89%-100.01%(RSD＝0.68%,n＝9). The content of samples were 1.920-2.018 mg/g. The contents of moisture in 3 batches of samples were 1.54%,1.62% and 1.57%;all samples dissolved within 5 min. The sum of granules not passing through No.1 sieve and passing through No.5 sieve were 2.13%, 2.51%,2.38%,which were all in line with the requirements of Chinese Pharmacopeia (2015 edition,Vol Ⅳ). CONCLUSIONS:The content of total flavonoicle in Chailing hugan granules should be no less than 1.57 mg/g (by rutin). Established quality standard is simple,rapid,accurate and reproducible,and can be used for quality control of Chailing hugan granules.

Optimization of quantitative method for curcumin and its carrier drugs by ultraviolet-visible spectrophotometry / 国际药学研究杂志

Objective To set up a convenient and rapid quantitative method for curcumin and its carrier drugs by ultraviolet-visible spectrophotometry. Methods Alkali-soluble method was used to determine the content of curcumin in its drug carriers. A certain amount of drug carriers containing curcumin was dissolved in 10 g/L sodium hydroxide solution and measured at maximum adsorption wavelength of 470 nm. The encapsulation ratio of drug carriers was determined according to the result of measurement using a calibration curve as a reference. Results The concentration (x) and absorbance (y) had a good linear correlation in the range of 8.0-15.0 mg/L. The regression equation was as follows: y=0.139x+0.009,r2=0.999 (n=7). The deviation was less than 0.4 mg/L within an hour. Conclusion This method is simple, rapid and accurate, with no pollution to the environment, which can be used for the entrapment efficiency and quality standards of curcumin nanoparticles.

Similarity Evaluation of the Dissolution Curves of Generic and Original Preparation of Losartan Potassium Tablets / 中国药房

OBJECTIVE:To evaluate the dissolution curves similarity of generic and original preparation of Losartan potassium tablets,and to provide reference for improving quality evaluation of the preparation.METHODS:Using hydrochloric acid solution (pH 3.0),phosphate buffer solution(pH 4.5),phosphate buffer solution (pH 6.8) and water as medium,paddle method was adopted for dissolution test with dissolution medium volume of 900 mL and rotation speed of 50 r/min.UV-visible spectrophotometry was adopted to determine accumulative dissolution of generic and original preparation of Losartan potassium tablets with the detection wavelength of 256 um.The similarity of dissolution curves were evaluated by calculating similarity factor(f2).RESULTS:The linear range of losartan potassium was 12.11-35.96 μg/mL (r≥0.999 7).RSDs of precision,stability and reproducibility tests were all lower than 5.0％.The recoveries of 4 dissolution media were 98.66％-100.84％ (RSD=0.77％,n=9),98.91％-100.59％ (RSD=0.49％,n=9),98.33％-101.39％ (RSD=0.85％,n=9),99.46％-101.32％ (RSD=0.55％,n=9).In 4 dissolution media,f2 of the dissolution curves of 3 batches of generic and original preparation of Losartan potassium tablets were all higher than 70.CONCLUSIONS:The dissolution curves of self-made and original preparation of Losartan potassium tablets show good similarity.

Determination of polymethoxylated flavones in Citri Reticulatae Pericarpium from eleven cultivar origins / 中成药

AIM To determine the contents of polymethoxylated flavones in Citri Reticulatae Pericarpium from eleven cultivar origins.METHODS HPLC was applied to screening extraction solvents (methanol,anhydrous ethanol,95％ ethanol,ethyl acetate and petroleum ether).Ultraviolet-visible spectrophotometry was adopted in the content determination of polymethoxylated flavones in eighteen batches of samples,nobiletin was taken as a reference substance,and the detection wavelength was set at 330 nm.RESULTS Ethyl acetate exhibited the best extraction effect,so it was selected as extraction solvent.Nobiletin showed a good linear relationship within the range of 3.024-13.104 μg/mL (R2 =0.999 8),whose average recovery was 101.37％ with the RSD of 1.34％.The contents of polymethoxylated flavones had obvious differences among samples from different cultivar origins,which were relatively high from Citrus reticulata ‘ Chachi’,Citrus reticulata ‘ Dahongpao’,Citrus reticulata ‘ Tangerina’,Citrus reticulata ‘ Ponkan’,Citrus reticulata ‘ Kinokuni’and Citrus reticulata ‘ Shiyueju’(more than 0.4％).CONCLUSION This simple and accurate method can effectively eliminate the interference of another flavonoids,which is suitable for the content determination of polymethoxylated flavones in Citri Reticulatae Pericarpium.

Optimization of quantitative method for curcumin and its carrier drugs by ultraviolet-visible spectrophotometry / 国际药学研究杂志

Objective To set up a convenient and rapid quantitative method for curcumin and its carrier drugs by ultraviolet-visible spectrophotometry. Methods Alkali-soluble method was used to determine the content of curcumin in its drug carriers. A cer?tain amount of drug carriers containing curcumin was dissolved in 10 g/L sodium hydroxide solution and measured at maximum adsorp?tion wavelength of 470 nm. The encapsulation ratio of drug carriers was determined according to the result of measurement using a cali?bration curve as a reference. Results The concentration(x)and absorbance(y)had a good linear correlation in the range of 8.0-15.0 mg/L. The regression equation was as follows:y=0.139x+0.009,r2=0.999(n=7). The deviation was less than 0.4 mg/L within an hour. Conclusion This method is simple,rapid and accurate,with no pollution to the environment,which can be used for the entrap?ment efficiency and quality standards of curcumin nanoparticles.

Elaboración de bio-resina intercambiadora de cationes a partir de cáscara de plátano o guineo para eliminar metales pesados en agua contaminada / Manufacture of cation exchange bio-resin from banana peel to remove heavy metals in contaminated water

Esta investigación tuvo por objetivo obtener una bio-resina intercambiadora de cationes utilizando cáscaras de guineo o plátano, la cual reduzca la concentración de metales pesados en agua contaminada. A esta bio-resina se le realizaron pruebas fisicoquímicas: densidad seca aparente, pH y solubilidad en agua y solventes orgánicos. Se evaluó su efectividad filtrando agua contaminada con metales pesados, tales como hierro, cromo y níquel (Fe3+, Cr6+ y Ni2+), variando las condiciones de tiempo de contacto, temperatura y el tipo de cáscara. La cuantificación de la concentración de los metales en el agua filtrada se llevó a cabo por espectrofotometría visible. Se llegó a la conclusión que la bio-resina obtenida es efectiva para disminuir la concentración de metales pesados en agua, teniendo especial afinidad química por el cromo hexavalente; metal pesado que logró remover arriba del 90%. Las condiciones óptimas de operación de la bio-resina son a 30°C y 90 minutos de tiempo de contacto con la muestra. Además, las pruebas fisicoquímicas, permitieron tipificarla preliminarmente como una resina de intercambio catiónico débil con un grado de entrecruzamiento bajo.

The objective of this research was to obtain a cation exchange bio-resin using banana peels, which reduces the concentration of heavy metals in contaminated water. Physicochemical tests were carried out on this bio-resin: apparent dry density, pH and solubility in water and organic solvents. Its effectiveness was evaluated by filtering water contaminated with heavy metals, such as iron, chromium and nickel (Fe3 +, Cr6 + and Ni2 +), varying the conditions of contact time, temperature and the type of shell. The quantification of the metal concentration in the filtered water was carried out by visible spectrophotometry. It was concluded that the bio-resin obtained is effective in reducing the concentration of heavy metals in water, having a special chemical affinity for hexavalent chromium; heavy metal that was able to remove over 90%. The optimal operating conditions for the bio-resin are at 30 ° C and 90 minutes of contact time with the sample. Furthermore, physicochemical tests allowed it to be preliminarily typified as a weak cation exchange resin with a low degree of crosslinking.

Chem ical Evaluation of Germplasm Resources of Paris Polyphylla var. Yunnanensis in Yunnan and Guizhou / 中国药师

Objective:To screen fine germplasm resources and suitable cultivated place for Paris polypyh lla var.yunnanensis by determining the content of total saponins , total flavonoids and total polysaccharides collected from Yunnan and Guizhou .Methods:An Ultraviolet-visible spectrophotometry method was applied to determine the total contents of saponin , flavonoid and polysaccharide in 14 germplasm resources of Paris polyhp ylla var.yunnanensis.Results:The contents of saponins, flavonoids and polysaccharides in Paris polyphylla var.yunnanensis collected from the different habitats were obviously different .The herb with high quality was selected from Xiaguan and Dali with the highest total content of saponins and the content of the three components was 55.760 0 and 61.632 0 mg· g-1 , respectively , which was significantly higher than that from the other habitats .Conclusion: It is proved that the quality of Pa ris polyphyll a var.yunnanensis produced in Dali of Yunnan is better than that from the other regions , and the high yield culture techniques should be studied further .

Study on Determination Method of Total Flavonoids in Gansu Astragali Radix and ;Hedysarum Polybotrys / 中国中医药信息杂志

Objective To study the determination method of total flavonoids in Gansu Astragali Radix and Hedysarum Polybotrys. Methods Calycosin glycosides etc. was selected as reference substances, comparison on the difference of absorption curves was done by ultraviolet spectroscopy and colorimetric method (NaNO2-Al(NO3)3-NaOH, AlCl3, Mg(Ac)2, NaOH, phosphomolybdic acid, HCl-Mg power). Results With colorimetric method, the maximum absorption wavelength of referrence and the test was inconsistent. The absorption peak shape was also different. With UV method, Calycosin glycosides in band Ⅱ (260 nm) showed a shoulder absorption. Astragali Radix and Hedysarum Polybotrys also showed characteristic shoulder absorptions in band Ⅱ with absorption wavelength at 263 nm and 265 nm. So the sample absorption wavelength is basically the same as that of the control sample. Conclusion Colorimetries usually used for determination of total flavonoids are not suitable for the comparison determination of Gansu Astragali Radix and Hedysarum Polybotrys. It is suitable for determining the contents of total flavonoids in samples by UV spectrophotometry at the band Ⅱ, which is the characteristic absorption band of isoflavone compound.

Determination of Total Saponins in Paridis Rhizome from Wudang Mountain Area by Ultraviolet-visible Spectrophotometry / 中国药师

Objective:To compare the content of total saponins in Paridis Rhizome from Wudang mountain area to explore the cor-relation between the quality of medicinal materials and the production areas and species. Methods: The content of total saponins in Paridis Rhizome was determined by an ultraviolet-visible spectrophotometer at 406nm with perchloric acid as the chromogenic reagent. Results:The saponins content in Paridis Rhizome from Wudang mountain area had obvious differences:the minimum was 1. 29%, and the maximum was up to 10. 22%. The content of total saponins had no obvious correlation with species, production area and altitude. Conclusion:The quality of Paridis Rhizome is unstable in Wudang mountain area, and that will affect the effectiveness and safety of the clinical medication. Only by promoting the standardized planting of Chinese medicine materials, the stable quality of Paridis Rhizo-me can be ensured.

β-Cyclodextrin-cross-linked Polymer Coupled Ultraviolet-Visble Spectrophotometry for Separation and Analysis of p-Nitrophenol / 分析化学

The β-cyclodextrin cross-linked polymer(β-CDCP) was used as adsorbent to pre-concentrate/separate the trace p-nitrophenol and then the determination was carried by UV-Vis spectrophotometry. Under alkaline condition,the adsorption/elution behavior of p-nitrophenol was studied. In 0. 02 mol/L NaOH solution and at room temperature for 30 min,the resin could separate and pre-concentrate the p-nitrophenol effectively. Methanol solution(1:1,V/V) was used as eluent and the β-CDCP could be used repeatedly. The linear range and detection limit was 0.5 -90.0 mg/L and 3. 10 μg/L,respectively. The proposed method has been used to determine the p-nitrophenol in synthesized sample with satisfactory results.

Preparation and Quality Control of Nicotinamide Gel / 中国药房

OBJECTIVE: To prepare Nicotinamide gel and to establish its quality control method.METHODS: Nicotinamide gel was prepared using nicotinamide as main ingredient,and the content of nicotinamide was determined by UV-visible spectrophotometry.RESULTS: Preparation was colorless gel,and its identification and test were all in conformity with the related regulation stated in Chinese Pharmacopoeia(2010 edition).The linear range of nicotinamide was 6.24～16.64 ?g?mL-1(r=0.999 5) with an average recovery rate of 102.0%(RSD=0.33%,n=5).CONCLUSION: The preparation procedure is simple and feasible,and the quality of the preparation is stable and controllable.

UV-Visible Spectrophotometric Assay for Saikosaponins in Bupleurum Chinense DC / 医学研究杂志

Objective To set up a simple and accurate method for the determination of saikosaponins in Bupleurum chinense DC. by UV-Visible Spectrophotometry. Methods The content of saikosaponins was determined by UV-Visible Spectrophotometry. The absorbency was measured at 536nm. Results The calibration curves was linear within 194~1940mg/L(r=0.9996). The average recovery was 97.35%,and the RSD was 1.02%(n=9). Conclusion The method was proved to be simple, precise and reproduciable. It can be used for the quantitative determination of B upleurum chinense DC.

Preparation and Quality Control of Compound Yolk Emulsion / 中国药房

OBJECTIVE:To prepare compound yolk emulsion and to establish its quality control method.METHODS:Compound yolk emulsion was prepared by emulsification.Cod liver oil and Nystalin in compound yolk emulsion were identified by color reaction and TLC,respectively.The content of VitB2 was determined by visible spectrophotometric method.The stability of 3 batches of samples was investigated as well.RESULTS:The linear range of VitB2 were 0.0 119～ 0.0 238 mg/ml(r=0.9 958).The average recovery of VitB2 was 97.95%(RSD=3.45%).3 batches of sample preparations were tested to be stable in quality at 4℃ ～ 8℃.CONCLUSION:This method is simple in operation,accurate in content determination,and stable and controllable in quality within expiration date.

Determination of Zedoary turmeric oil microsphere / 中成药

AIM: To study a method for the determination of Zedoary turmeric oil microsphere (ZTO-MS). METHODS: ZTO-MS was extracted supersonically by solvent and then colored by sulfuric acid-vanillin reagent. The absorbance was measured by visible-spectrophotometry at 508nm. At the same time, ZTO-MS also could be determined by HPLC. RESULTS: The content of Zedoary turmeric oil was above 60% and the contents of Curdione、Curcuma、Germacrone were 6.88%,0.95%,5.0%, respectively, in ZTO-MS. CONCLUSION: Two methods for the determination of ZTO-MS are accurate, reliable; the method of visible-spectrophotometry is convenient and appropriate for determination for content of oil in ZTO-MS, while the method of HPLC gains the advantage for qualitative and quantitative analysis of components in ZTO-MS.