Determination of total polyphenols and catechins in betel nut polyphenol extract / 药学实践杂志

Objective To establish a method for the determination of total polyphenols and catechins in betel nut polyphenols extract, and provide reference for the quality control of betel nut polyphenols extract. Methods The content of total phenol in betel nut extract was determined by ultraviolet spectrophotometry. The content of catechins was determined by HPLC. Results The linear range of total polyphenols in betel nuts extract was 9.8~58.8 μg/ml. The three components of catechin, epicatechin and protocatechuic acid were completely separated by HPLC, and the linear relationship was good in their respective ranges, with the recoveries between 99.17% and 101.67%, the RSD between 1.2% and 2.5%. Conclusion The established method is simple, stable and reliable, which could be used for the quantitative analysis of betel polyphenol extract, and provide experimental basis for the quality control of betel polyphenol extract.

Study on the determination of total flavonoids in Oxytropis falcata Bunge / 药学实践杂志

Objective To establish an UV spectrophotometry method for the determination of total flavonoids in Oxytropis falcata Bunge. Methods Using rutin as comparison，three coloration methods were used to find the optimal assay method, optimize the color conditions and take a systematic methodological investigation. Results The best color development method is aluminum chloride-sodium acetate color method. Using the test product without adding color reagent as a reference, 0.3 mol/L aluminum chloride solution 3.0 ml, 1.0 mol/L sodium acetate 4.0 ml, placed for 16 min, the sample was detected at 277 nm wavelength by AlCl3-CH3COONa reaction by using rutin as reference. The rutin content had a good liner relationship in the range of 8.8 to 44 μg/ml (r=0.9996), and the average recovery rate was 100.91% with RSD of 2.426%. Conclusion This method is simple, rapid, accurate and sensitive and can be used as a method for the determination of total flavonoids from Oxytropis falcata Bunge.

Optimization of the Extraction Technology of Total Flavonoids from Combretum alfrdii / 中国药房

OBJECTIVE： To establish the method for content determination of total flavonoids from Combretum alfrdii， and to optimize the extraction technology of total flavonoids from C. alfrdii. METHODS： Using aluminium trichloride as， chromogenic agent， UV spectrum was adopted to determine the content of total flavonoids from C. alfrdii. Based on single factor test， ethanol volume fraction， material-liquid ratio， extraction time， extraction temperature and times were selected as investigation factors， and the content of total flavonoids was selected as response value， Plackett-Burman design was used to screen the factors that had significant influence on the content of total flavonoidsfrom C. alfrdii. Then steepest climbing test was adopted to confirm the optimum valuing range； the extraction technology of total flavonoids was optimized by Box-Behnken response methodology. RESULTS： The linear range of total flavonoids were 0.012-0.036 mg/mL （r＝0.999 9）； RSDs of precision， stability and repeatability tests were less than 3％； the recovery ranged from 92.98％ to 99.86％ （RSD＝2.71％， n＝6）. The optimal extraction technology included that 60％ ethanol， material-liquid ratio of 1 ∶ 34 （g/mL）， extracting for 3 times， lasting for 60 min， extraction temperature of 80 ℃. Under this technology， average content of total flavonoids from C. alfrdii was 2.71％ （RSD＝1.69％， n＝6）， and the relative error was 2.65％ compared with predicted value of the model （2.64％）. CONCLUSIONS： Established method is stable and reproducible， and can be used for content determination of total flavonoids from C. alfrdii. The optimized extraction method is stable and feasible.

Optimization of the Preparation Technology of Syzygium aromaticum Oil Dropping Pills / 中国药房

OBJECTIVE： To establish the method for content determination of eugenol in Syzygium aromaticum oil dropping pills， and to optimize the preparation technology. METHODS： The content of eugenol in S. aromaticum oil dropping pills was determined by UV spectrophotometry. Based on single factor test， using the percentage of drugs in total amount， liquid temperature， falling distance of condensate， liquid drop distance as factors， taking the roundness， weight and hardness difference and comprehensive score as factors， L9（34） orthogonal design test was adopted to optimize the preparation process. RESULTS： The linear range of eugenol was 15.15-45.45 μg/mL（r＝0.999 6）； RSDs of precision， stability and reproducibility tests were all lower than 1％； the recoveries were 97.41％-100.59％（RSD＝1.35％， n＝6）. The optimal preparation technology included that the percentage of drugs in total amount was 5％； liquid temperature was 80 ℃； falling distance of condensate was 13 cm； liquid drop distance was 6 cm. The dropping pills had smooth appearance， good roundness and moderate hardness； the average content of engenol was 4.073％（RSD＝0.35％，n＝6）. CONCLUSIONS： The established method is simple， and can be used for the content determination of eugenol in S. aromaticum oil dropping pills. The optimal preparation technology is stable and feasible.

Optimization of the Extraction Technology of Total Flavonoids from Typhonium divaricatum / 中国药房

OBJECTIVE： To establish a method for the content determination of total flavonoids from Typhonium divaricatum， and to optimize its extraction technology. METHODS： The content of total flavonoids in T. divaricatum was determined by UV spectrophotometry. Using the extraction amount of total flavonoids from T. divaricatum as index， the volume fraction of ethanol， the ratio of material to liquid， the extraction time and times as factors， the extraction technology of total flavonoids from T. divaricatum was optimized by L9（34） orthogonal design， based on the single factor test. RESULTS： The linear range of rutin were 8-48 μg/mL （r＝0.999 7）； the quantification limit was 0.54 μg/mL， and the detection limit was 0.18 μg/mL； RSDs of precision， stability and repeatability tests were all lower than 2％. The recoveries were 99.61％-102.38％（RSD＝1.15％， n＝6）. The optimal extraction technology was as follows： ethanol concentration of 70％， solid-liquid ratio of 1 ∶ 20 （g/mL）， extraction time of 45 min， extracting for 2 times. Under this condition， the average content of total flavonoids from T. divaricatum was 2.74 mg/g.  CONCLUSIONS： Established method is simple and accurate； the extraction process is stable and feasible.

Study on Quality Standard of Bushen Quyu Granules / 中国药房

OBJECTIVE： To establish the quality standard for Bushen quyu granules. METHODS： TLC was used for qualitative identification of Rosa laevigata， Cuscuta chinensis， processed Fallopia multiflora and Lithospermum erythrorhizon in Bushen quyu granules. And then， the content of total polysaccharides in Bushen quyu granules was determined by UV spectrophotometry. HPLC method was used for the content determination of rutin， quercetin and hyperin in Bushen quyu granules. The determination was performed on BDS C18 column with mobile phase consisted of acetonitrile-0.08％ phosphoric acid solution （gradient elution） at the flow rate of 1 mL/min. The column temperature was 30 ℃， and detection wavelength was set at 370 nm. The sample size was 10 μL. RESULTS： TLC test sample chromatogram of 4 medicinal materials showed the same spot or fluorescence at the corresponding position with the reference substance and control medicinal materials. The linear range of glucose， rutin， quercetin and hyperin were 0.003-0.018 mg/mL， 0.225-7.20 μg/mL， 0.07-2.24 μg/mL and 1.25-39.88 μg/mL（r＝0.999 5 or 0.999 9， n＝6）. RSDs of precision， stability and reproducibility tests were all less than 3％ （n＝6）. Average recoveries were 102.2％， 101.2％， 100.9％， 101.0％ （RSD＝1.28％， 2.93％， 2.41％， 1.59％， n＝6）. Average contents were 0.46 g/g， 5.48        μg/g， 8.18 μg/g and 102.88 μg/g（n＝3）. CONCLUSIONS： Established quality standard of Bushen quyu granules is accurate and reliable， and can provide scientific reference for quality control of Bushen quyu granules.

Evaluation of Measurement Uncertainty for the Determination of Flavonoids in Loquat Honey by UV Spectrophotometry / 医药导报

Objective To evaluate the measurement uncertainty of flavonoids in loquat honey by UV spectrophotometry. Methods Through analyzing the whole process of the total flavonoids in loquat honey by UV spectrophotometry detection,the mathematical model was established,the uncertainty factors were determined,and each uncertainty was evaluated.Then the combined uncertainty was calculated and the expanded uncertainty of the measurement results at the 95％ confidence interval was given. Results The measurement uncertainty of the totle flavonoids content in loquat honey by UV spectrophotometry was (38.497±5. 674) μg?g-1 . Conclusion The uncertainty evaluation method is suitable for determination of the total flavonoids in loquat honey by UV method,and the uncertainty is mainly introduced by preparation of reference stock solution and standard curve fitting.

Decoction of Isoflavone Content and Its Acid Hydrolysis Conversion Rate in the Flower of Pueraria lobata / 中国药房

OBJECTIVE:To establish a method for the decoction of isoflavone content and its acid hydrolysis conversion rate in the flower of Pueraria lobata. METHODS:Using the flowers of Pueraria lobata as raw material,the isoflavone with main com-ponent of tectoridin in the flower of P. lobata was prepared with ethanol,ethyl acetate extracted,ethanol recrystallized and puri-fied,and it was converted to tectorigenin with hydrolysis in hydrochloric acid. By screening the solvent and wavelength,UV spec-trophotometry was established to determine tectovidin and tectorigenin,and calculate the isoflavone content and acid hydrolysis con-version rate of tectoridin(expressed by the relative percentage of tectorigenin). It was compared with HPLC detection results,the accuracy of UV method was evaluated. RESULTS:The solvent was 70％ethanol solution containing 1％triethylamine,and the iso-flavone content was detected at wavelength of 339,274 nm. The linear range of tectoridin was 8.80-29.33 nmol/mL(r=0.9999). RSDs of precision(n=6),stability(n=5)and reproducibility(n=6)tests were lower than 1.94％;average recovery was 99.7％(RSD=1.77％,n=9). There were no statistical significances in the contents of total flavonoids (UV:17.64-25.55 nmol/mL vs. HPLC:17.39-24.40 nmol/mL) and the relative percentage of tectorigenin (UV:57.65％-87.59％ vs. HPLC:55.62％-91.14％). CONCLUSIONS:The established method is accurate,reliable,and can be used for the rapid determination of acid hydrolysis con-version rate of tectoridin.

Quality control and physico-chemical properties of vitamin K1 self-nanoemulsifying drug delivery systems / 国际药学研究杂志

Objective To establish assay methods for the determination of dissolution,content and related substances of vita-min K1 self-nanoemulsifying drug delivery system(VK1-SNEDDS),and investigate the physico-chemical properties of the preparation. Methods The UV method was established to determine the dissolution of VK1-SNEDDS. The content and related substances were de-termined by HPLC. The appearance,self-emulsification time,micro-morphology,droplet size and zeta potential were also investigat-ed. Results The linearity range of established UV and HPLC methods was 0.85-20.4 and 2.16-216μg/ml,respectively,and all the recovery,precision,specificity and sensitivity met requirements. VK1-SNEDDS could disperse quickly after dilution. The transmission electron microscope(TEM)image of the optimized liquid SNEDDS showed that most of the emulsion droplets were of uniform size with no signs of coalescence. Droplet size of optimal formulation was revealed as 47.74 nm with polydispersibility index(PDI)of 0.248,and zeta potential was found to be-20.53 mV. Conclusion VK1-SNEDDS could form homogeneous and stable nanoemulsion when dilut-ed with aqueous phase and increase the dissolution of lipophilic drug. The methods are reliable,accurate and suitable for quality con-trol of VK1-SNEDDS.

Research on the determination of total flavonoids in compound Yinchen mixture / 药学实践杂志

Objective To establish a method for the determination of the total flavonoids content in compound Yinchen mixture by UV spectrophotometry .Methods Using rutin as comparison ,three coloration methods were studied to find the op-timal assay method .Results The sample was detected at 508 nm wavelength by NaNO2-Al(NO3 )3-NaOH reaction with rutin as reference .The rutin content had a liner relationship in the range of 0 .0125-0 .0626 g/L (n=9 ,r=0 .9999) ,and the aver-age recovery rate was 99 .49％ with RSD of 0 .84％ .Conclusion The NaNO2-Al(NO3 )3-NaOH coloration method is proved to be simple ,quick ,stable and reliable for the determination of total flavonoids in compound Yinchen mixture .

The methodology validation and content assay of total polysaccharides in Pudi Enema / 药学实践杂志

Objective To establish the assay method for the total polysaccharide in Pudi Enema.Methods Phenol-sulfuric acid method was used for chromogenic reaction.The content of total polysaccharide was measured by UV spectrophotometry at 488.8 nm.Results The total polysaccharides calibration curve was at the range of 0~22.635 mg/L, with regression function being Y=0.062 06 X-0.003 34(r=0.999 8).The recovery of calycosin was 98.36%(RSD=2.34%).Conclusion This method is sensitive,rapid,accurate and reliable.It can be used to assay the content of total polysaccharide in Pudi Enema.

Determination of amlodipine and telmisartan in the compound tablet by first de-rivative UV spectrophotometry / 药学实践杂志

Objective To determine telmisartan and amlodipine assay in the compound tablet .Methods First derivative UV spectrophotometry was used at wavelength 236 nm for telmisartan and 390 nm for amlodipine .Results Telmisartan con-tent has a good linear relationship in the concentration range of (4~20) × 10-3 mg/ml .The standard curve equation is Y =0 .0043 X-0 .0005 and correlation coefficient R2 =0 .9993 .Amlodipine content has a good linear relationship in the concen-tration range of (10~90) × 10-3 mg/ml .The standard curve equation is Y =0 .0003 X+0 .0002 and correlation coefficient R2 =0 .9995 .Conclusion The assay results from this method are consistent with the results from HPLC .This procedure pro-vides a specific ,accurate and precise method to assay the amlodipine and telmisartan in compound tablet .

Determination of Erythromycin in Erythromycin Enteric Capsules by UV / 中国药师

Objective:To establish a method for the determination of erythromycin in erythromycin enteric capsules. Methods:UV spectrophotometry was performed. Sodium hydroxide reacted with erythromycin to obtain a unsaturated ketone having maximum absor-bance at 235 nm. The content of erythromycin in erythromycin enteric capsules was determined by the UV absorbance of the unsaturat-ed ketone. Results: The linear range of erythromycin was 51. 18-307. 08 μg · ml-1 ( r =0. 999 9 ) and the average recovery was 99. 9%(RSD=1. 2%,n=6). Conclusion:The method is simple,accurate,sensitive and reproducible, which can be used for the de-termination of erythromycin in erythromycin enteric capsules.

Effects of Particle Size of Ticagrelor Crude Drug on in vitro Dissolution Behavior of Ticagrelor Tablets / 中国药房

OBJECTIVE:To study the effects of particle size of ticagrelor crude drug on in vitro dissolution behavior of Ticagre-lor tablets. METHODS:Ticagrelor crude drug and different particle size of ticagrelor powder A,B,C,D,E after smashing for dif-ferent time(15,30,40,60 s)were used to prepare the tablet by wet granulation method. Accumulative in vitro dissolution rate of prepared tablets within 60 min were determined by UV spectrophotometry at 300 nm(using 0.2% tween as medium,paddle meth-od). Using original tablet as reference preparation,the similarity factor(f2)method was used to compare the similarity of dissolu-tion behavior between 5 prepared tablets and original tablet. RESULTS:d(0.9)of powder A,B,C,D,E were 69.181,40.778, 24.805,12.611,3.083 μm,respectively. The corresponding f2 were 27.77,36.79,50.06,67.68,79.99. CONCLUSIONS:The par-ticle size of ticagrelor crude drug is much smaller,and the dissolution behavior of prepared tablet is closer to that of original tablet. The in vitro dissolution rate of Ticagrelor tablets is improved remarkably by micronization technology. In order to produce Ticagre-lor tablets with the same bioavailability as original tablet,particle size of ticagrelor crude drug powder should be controlled with d(0.9)≤20μm.

New qualities control strategy of Scutellaria baicalensis by isothermal titration calorimetry / 中国中药杂志

It has been focused on that there will be precipitates when decoction of Scutellariat Radix mixed with Coptidis Rhizoma. Precipitation was derived from interaction between acidic and basic compounds. This study was based on the interaction between active ingredients after compatibility, strived to explore whether it was feasible to judge the qualities of different Scutellariat Radix by isothermal titration calorimetry (ITC), build a new method established to characterize the qualities of traditional Chinese medicine by taking a series of active ingredients as index. We selected Scutellariat Radix (including three batches of different Scutellariat Radix bought from market and immature Scutellariat Radix which usually was used as adulterant) in different batches as the samples. First, we used ITC to determine the binding heat of the reactions between berberine and the decoctions of different Scutellariat Radix. The test showed that the binding heat of berberine titrated Scutellariat Radix was Scutellariat Radix A (－317.20 μJ), Scutellariat Radix B (－292.83 μJ), Scutellariat Radix C (－208.95 μJ) and immature Scutellariat Radix (－21.53 μJ), respectively. We chose deionized water titrated by berberine (2.51 μJ) as control. The heat change of berberine titrated immature Scutellariat Radix was much less than berberine titrated Scutellariat Radix. Then we determined the absorbance of different decoctions of Scutellariat Radix by UV Spectrophotometry on the maximum absorption wavelength, and the result is： Scutellariat Radix A (0.372), Scutellariat Radix B (0.333), Scutellariat Radix C (0.272), immature Scutellariat Radix (0.124). The absorbance of immature Scutellariat Radix was also less than Scutellariat Radix. The result of ITC assay was corresponded to UV spectrophotometry test. In conclusion, ITC could be used to characterize the quality of Scutellariat Radix. The new method to characterize the qualities of traditional Chinese medicine by taking a kind of active ingredients as index building by ITC was simple, scientific and feasible.

The use of chitosan in protecting wooden artifacts from damage by mold fungi

Background: Many buildings in Egypt e.g. museums, mosques and churches, do not possess controlled environments for minimizing the risks of damage of wooden artifacts due to the growth of fungi. Fungal damage usually appears as change in wood color, appearance of stains, and sometimes deformation of wooden surfaces. In this study we focused on the effect that some fungi exert on the properties of wooden artifacts and evaluated the effectiveness of different concentrations of chitosan on their protection against damage by mold fungi. Results: Samples were collected from different monuments and environments, and fungi growing on them were isolated and identified. The isolated Penicillium chrysogenum, Aspergillus flavus and /Aspergillus niger strains were used for the infestation of new pitch pine samples. The results revealed that the lightness of samples infected with any of the tested fungi decreased with increasing incubation times. XRD analysis showed that the crystallinity of incubated samples treated individually with the different concentrations of chitosan was lower than the crystallinity of infected samples. The crystallinity index measured by the first and the second method decreased after the first and second months but increased after the third and fourth months. This may due to the reducing of amorphous part by enzymes or acids produced by fungi in wooden samples. Conclusions: The growth of fungi on the treated wood samples decreased with increasing the concentration of chitosan. Hence, it was demonstrated that chitosan prevented fungal growth, and its use could be recommended for the protection of archeological wooden artifacts.

Validación del método espectrofotométrico para control de calidad de la colchicina en Artrichine tabletas / Validation of the spectrophotometric method for the quality control of Artrichine tablets

Introducción: la colchicina es una alternativa terapéutica indicada por vía oral para las crisis agudas de la gota. Se formula en tabletas de baja dosificación debido a su elevada toxicidad. Los Laboratorios Dr.A. Bjarner C.A producen las tabletas de Artrichine y se requiere de un método sencillo, pero a la vez confiable para realizar el control de calidad de este producto terminado, que considere la solubilidad en etanol, la presencia de cromóforos y la composición de la formulación de la colchicina. Objetivo: se propuso validar un método por espectrofotomería UV útil para el control de rutina. Métodos: se aplicó un método simple, que se modifica del método establecido en la Farmacopea Británica del 2009 para las tabletas, por espectrofotometría UV directa. Se basa en la extracción del analito en etanol absoluto y su posterior determinación a 350 nm. La validación del método se realizó a través de los parámetros linealidad, precisión, exactitud y especificidad frente a los componentes de la formulación. Resultados: se estableció una metodología analítica muy sencilla para obtener una solución transparente a partir de la forma terminada, de igual concentración a la solución de referencia. El cumplimiento satisfactorio de todos los criterios de aceptación establecidos para los parámetros evaluados permitió demostrar la validez del método en estudio para el control de calidad en el rango de 50 a 150 por ciento (5-15 µg/mL). Conclusiones: el método por espectrofotometría UV resultó específico, lineal, exacto y preciso para su aplicación al control de calidad de la colchicina en Artrichine tabletas(AU)

Introduction: colchicine is a therapeutic alternative orally prescribed for acute gout. It is formulated as low dose tables due to its high toxicity. Dr A. Bjarner C.A laboratories manufacture Artrichine tablets and it requires a simple and reliable method to conduct quality control of the finished product that will consider ethanol-soluble characteristics, presence of chromophores and composition of colchicine formulation. Objective: to validate an ultraviolet spectrophotometry-based method for the routine quality control. Methods: a simple method by direct UV spectrophotometry which is modified from the set method of the British Pharmacopeia 2009 for tablets. It is based on the analyte extraction in absolute ethanol and the estimation at 350 nm. The method was validated on account of linearity, precision, accuracy and specificity against the formulation components. Results: a very simple analytical methodology was established to obtain a transparent solution from the finished form, with the same concentration as that of the reference solution. The satisfactory compliance with all the acceptance criteria for the evaluated parameters allowed proving the validity of the study method for the quality control in the 50 to 150 percent range (5-15 ug/ml). Conclusions: the UV spectrophotometry-based method proved to be specific, linear, accurate and precise for the quality control of colchicine in Artrichine tablets(AU)

Quality control of desvenlafaxine succinate extended-release tablets / 国际药学研究杂志

Objective To establish and validate the assay methods of release, content, content uniformity and related substances of desvenlafaxine succinate (DVS) in extended- release tablets. Methods The ultraviolet spectrophotometric method was used to determine the DVS release from DVS extended-release tablets. The content uniformity, content and related substance were determined by high-performance liquid chromatography (HPLC). To validate all the method, we respectively examined specificity, linearity, recovery rate, precision and stability, etc. Results The results showed that the analysis method for release was specific, the calibration curve was linear in the range of 10-200 µg/ml, and all the recovery, repeatability and intermediate precision met requirements. The method for detection of content and content uniformity was specific and linear in the range of 5-400 µg/ml, the recovery, repeatability and intermediate precision met requirements. The method for related substances was specific and sensitive, the linear and recovery rate met the requirements. All of the solutions were stable during 24 h at room temperature. Conclusion The analysis method for release is simple, sensitive, specific and accurate, the method for content and content uniformity is accurate and reliable, and the method for related substances is specific, sensitive and accurate. These methods are suitable for quality control of DVS extendedrelease tablets.

Comparison of Two Methods for the Determination of Ciprofloxacin in Compound Cod-liver Oil Emulsion / 中国药师

Objective:To compare two methods for the determination of compound cod-liver oil emulsion. Methods:The content of ciprofloxacin in compound cod-liver oil emulsion was determined by HPLC and UV, respectively. The determination by HPLC was performed on a Thermo C18 column (150 mm ×4.6 mm, 5 μm). The mobile phase was 0.025 mol·L-1phosphate-acetonitrile (87∶13)andpHwasadjustedto3.0±0.1withtriethylamine. Thedetectionwavelengthwas277nmandtheflowratewas1.5ml·min-1. The detection wavelength of UV was 277 nm. Results:The average recovery of HPLC and UV was 100. 44% and 100. 84% with RSD of 1. 01% and 1. 09% (n=9), respectively. The detection results of the two methods were compared by paired sample t-test, and no statistically significant difference was found (P>0. 05). Conclusion:The two methods are specific and accurate, and can be used for the determination of ciprofloxacin hydrochloride in compound cod-liver oil emulsion.

Quality control of desvenlafaxine succinate extended-release tablets / 国际药学研究杂志

Objective To establish and validate the assay methods of release,content,content uniformity and related sub?stances of desvenlafaxine succinate (DVS) in extended-release tablets. Methods The ultraviolet spectrophotometric method was used to determine the DVS release from DVS extended-release tablets. The content uniformity,content and related substance were deter?mined by high-performance liquid chromatography(HPLC). To validate all the method,we respectively examined specificity,linearity, recovery rate,precision and stability,etc. Results The results showed that the analysis method for release was specific,the calibra?tion curve was linear in the range of 10-200μg/ml,and all the recovery,repeatability and intermediate precision met requirements. The method for detection of content and content uniformity was specific and linear in the range of 5-400μg/ml,the recovery,repeat?ability and intermediate precision met requirements. The method for related substances was specific and sensitive ,the linear and recovery rate met the requirements. All of the solutions were stable during 24 h at room temperature. Conclusion The analysis meth?od for release is simple,sensitive,specific and accurate,the method for content and content uniformity is accurate and reliable,and the method for related substances is specific,sensitive and accurate. These methods are suitable for quality control of DVS extended-release tablets.