Determination of Total Lignanoids in Tangjiangshenkang Granules by Two-Wavelength Ultraviolet Spectrophotometry

[Objectives] To establish a determination method for the content of total lignanoids in Tangjiangshenkang granules. [Methods] Two-wavelength ultraviolet spectrophotometry (TWBS) was used to scan arctiin control solution, chlorogenic acid control solution and Tangjiangshenkang granule test solution in the range of 200-400 nm. In the ultraviolet scanning diagram of arctiin reference solution, the maximum absorption wavelength of 280 nm was determined as the determination wavelength λ 1, the detection wavelength in the ultraviolet scanning diagram of chlorogenic acid reference solution ( λ 1=280 nm) was determined, and 350 nm was the reference wavelength λ 2;the content of total lignosides in Tangjiangshenkang granules was determined with arctiin as the reference substance. [Results] The precision, accuracy, and durability of this method were fine. The concentration of arctiin was linearly correlated with the absorbance difference in the range of 0.007 95-0.071 55 mg/mL ( r =0. 999 9). The average recovery of arctiin was 100.8%, and the RSD value was 1.04% ( n =6). Calculated as arctiin, three batches of Tangjiangshenkang granules contain no less than 20% of total lignosides. [Conclusions] The method has the advantages of simple operation, good accuracy, precision and reliable stability. It can be used as the content determination and quality control method of total lignosides in Tangjiangshenkang granules.

ULTRAVIOLET SPECTROPHOTOMETRY OF MULTI-COMPONENT MIXTURES USING ARTIFICIAL NEURAL NETWORKS

Three—layer back—propagation neural networks were used for processing the information provided by the ultraviolet spectra of five—component mixtures, affecting the simultaneous determination of the components with satisfactory results.

Two spectrophotometric methods for simultaneous determination of some antihyperlipidemic drugs

Two simple, accurate, precise and economic spectrophotometric methods have been developed for simultaneous determination of Atorvastatin calcium (ATR) and Ezetimibe (EZ) in their bulk powder and pharmaceutical dosage form. Method (I) is based on dual wavelength analysis while method (II) is the mean centering of ratio spectra spectrophotometric (MCR) method. In method (I), two wavelengths were selected for each drug in such a way that the difference in absorbance was zero for the second drug. At wavelengths 226.6 and 244 nm EZ had equal absorbance values; therefore, these two wavelengths have been used to determine ATR; on a similar basis 228.6 and 262.8 nm were selected to determine EZ in their binary mixtures. In method II, the absorption spectra of both ATR and EZ with different concentrations were recorded over the range 200-350, divided by the spectrum of suitable divisor of both ATR and EZ and then the obtained ratio spectra were mean centered. The concentrations of active components were then determined from the calibration graphs obtained by measuring the amplitudes at 215-260 nm (peak to peak) for both ATR and EZ. Accuracy and precision of the developed methods have been tested; in addition recovery studies have been carried out in order to confirm their accuracy. On the other hand, selectivities of the methods were tested by application for determination of different synthetic mixtures containing different ratios of the studied drugs. The developed methods have been successfully used for determination of ATR and EZ in their combined dosage form and statistical comparison of the developed methods with the reported spectrophotometric one using F and Student’s t-tests showed no significant difference regarding both accuracy and precision.

IMPROVEMENT OF FLUORIMETRIC AND UV－VISIBLE SPECTROPHOTOMETRIC ASSAY METHODS FOR MEASURING NITRIC OXIDE AND／OR EDRF IN BLOOD

The increasing importance of endothelium-derived relaxing factor(EDRF),which has now been identified as nitric oxide (NO),has been underscored by the eltlcidation of its role'in a growing number of normal and pathophysiological processes. Therefore techniques for detection of nitric oxide should serve as useful tools in defining the role of nitric oxide to these processes.We have improved a simple, sensitive assay methods for determination of nitric oxide in blood, tissue, and other body fluids both by fluorometric and by ultraviolet-visible spectrophotometric measurements. Data obtained by floores cence and by UV-visible assay were correlated well (r=0. 9938, P<0. 0001 ).Linearity:0.1￣ 100μmol/L,r =0.9996,P<0.0001. The minimum detection limit were < 10pmol/L. Within-and between-run CVs were 2. 48%and 4. 62% (n = 10),respectively.Reference values for healthy adults(n=40) were(9.82 ± 1. 57) pmol/L. In conclusion:the methods is sensitive, specific,and precise. It is fairly rapid and simple to perform andrequires no pretreatment of sample, i. e., plasma and urine.The value can be obtained by fluorimeter and/or UV-visible spectrophotometer.The present method is sufficiently rapid and simple to make this a practical choice for many laboratories.

Simple Spectrophotometric Methods for the Determination of Meloxicam in Presence of Its Degradation Products

To develope two simple and accurate spectrophotometric methods for the determination of meloxicam( I )in presence of its degradation products, 5 -methyl -2 -aminothiazole ( II )and benzothiazine carboxylic acid( Ill ). Method:Both methods are based on the formation of chelate complexes of the studied drug with uranyl acetate and ferric chloride at room temperature in a methanolic medium. Results:The resulting complexes are stable for 24 hrs and show absorption maxima at 406 nm and 580 nm for uranyl and ferric complexes respectively. These methods are applicable over the concentration ranges of 10 -100 and 37.5 -300 p^g ~ mL-1 with mean recoveries of (99.44 ~ 0. 48 ) % and (99. 42 ~ 0. 45 ) %, and molar absorptivity of 4.67 x 103 and 1. 029 x 103 respectively. Conclusion:Both methods are proved to be stability indicating as no interference was observed with the degradation products. The proposed methods were successfully applied to the determination of the frug in bulk powder, laboratory prepared mixtures containing different percentages of degradation products of the drug in bulk powand pharmaceutical dosage

Validated stability indicating methods for determination of nitazoxanide in presence of its degradation products

Three sensitive,selective and reproducible stability-indicating methods are presented for determination of nitazoxanide (NTZ),a new anti-protozoal drug,in presence of its degradation products.Method A utilizes the first derivative of ratio spectra spectrophotometry by measurement of the amplitude at 364.4 nm using one of the degradation products as a divisor.Method B is a chemometric-assisted spectrophotometry,where principal component regression (PCR) and partial least squares (PLS) were applied.These two approaches were successfully applied to quantify NTZ in presence of degradation products using the information included in the absorption spectra in the range 260-360 nm.Method C is based on the separation of NTZ from its degradation products followed by densitometric measurement of the bands at 254 nm.The separation was carried out on silica gel 60F 254,using chloroform-methanol-ammonia solution-glacial acetic acid (95:5:1:1 by volume,pH=5.80) as a developing system.These methods are suitable as stability-indicating methods for the determination of NTZ in presence of its degradation products either in bulk powder or in pharmaceutical formulations.Statistical analysis of the results has been carried out revealing high accuracy and good precision.

Effects of Different Preservation Methods on Vitamin C and Nitrate Content in Vegetables

This paper studied and compared the effects of three preservation methods( normal temperature 20℃,fresh-keeping box cold storage 4℃,and fresh-keeping box + fresh-keeping film cold storage 4℃) on six kinds of vegetables. The results showed that the content of vitamin C in the six vegetables was higher in cold storage than in normal temperature storage; the nitrate content was lower in cold storage than in normal temperature storage. In both the normal temperature storage and cold storage,the vitamin C in vegetables declined with the increase of the storage time,while the nitrate content increased with the increase of the storage time. Thus,cold storage has better fresh-keeping effect for vegetables. In cold storage conditions,the vitamin C content was higher in vegetables packaged by fresh-keeping box,and the nitrate content was lower,followed by the fresh-keeping film + fresh-keeping box cold storage. In conclusion,the best preservation method for vegetable is fresh-keeping box cold storage.

Mechanistic Study and Kinetic Determination of Cu(Ⅱ) by the Catalytic Kinetic Spectrophotometric Method

A highly sensitive and selective catalytic kinetic spectrophotometric method for the determination of Cu(Ⅱ) is proposed. It is based on the catalytic effect of Cu(Ⅱ) on the oxidation of glutathione(GSH) by potassium hexacyanoferrate(Ⅲ) in acidic medium at 25.0℃. The reaction is monitored spectrophotometrically by measuring the decrease in absorbance of oxidant at 420 nm using the fix-time method. Under the optimum conditions, the proposed method allows the determination of Cu(Ⅱ) in a range of 0-35.0 ng m L^(-1) with good precision and accuracy and the limit of detection is down to 0.04 ng m L^(-1). The relative standard deviation(RSD) is 1.02%. The reaction orders with respect to each reagent are found to be 1, 1/2, and 1/2 for potassium hexacyanoferrate(Ⅲ), glutathione and Cu(Ⅱ) respectively. On the basis of these values, the rate equation is obtained and the possible mechanism is established. Moreover, few anions and cations can interfere with the determination of Cu(Ⅱ). The new proposed method can be successfully used to the determination of Cu(Ⅱ) in fresh water samples and seawater samples. It is found that the proposed method has fairly good selectivity, high sensitivity, good repeatability, simplicity and rapidity.

Establishment of the Determination Methods of Total Anthraquinone Content in Different Processed Products of Rhubarb

[Objectives]Ultraviolet spectrophotometry was established for the determination of total content of anthraquinone in different processed products of rhubarb.[Methods]Emodin was used as the control substance,and its color was developed by magnesium acetate methanol solution with the concentration of 1%,the absorbance was determined at the wavelength of 516 nm,the content of total anthraquinone in different processed products of rhubarb was determined to compare the content differences.[Results]The regression equation was y=0.0452 x+0.0015,R 2=0.9991.Emodin had a good linear range in the concentration of 0.98-23.52μg/mL,with high accuracy,good repeatability and stable detection results.This method revealed the content changes of total anthraquinone in rhubarb before and after processing.[Conclusions]This method could be used as the quality control method of different processed products of rhubarb,and provided reference for the comprehensive development and utilization of rhubarb resources in the future.

Simplified quantitative analysis method and its application in the insitu synthesized copper-based azide chips

Copper-based azide(Cu(N_(3))2 or CuN_(3),CA)chips synthesized by in-situ azide reaction and utilized in miniaturized explosive systems has become a hot research topic in recent years.However,the advantages of in-situ synthesis method,including small size and low dosage,bring about difficulties in quantitative analysis and differences in ignition capabilities of CA chips.The aim of present work is to develop a simplified quantitative analysis method for accurate and safe analysis of components in CA chips to evaluate and investigate the corresponding ignition ability.In this work,Cu(N_(3))2 and CuN_(3)components in CA chips were separated through dissolution and distillation by utilizing the difference in solubility and corresponding content was obtained by measuring N_(3)-concentration through spectrophotometry.The spectrophotometry method was optimized by studying influencing factors and the recovery rate of different separation methods was studied,ensuring the accuracy and reproducibility of test results.The optimized method is linear in range from 1.0-25.0 mg/L,with a correlation coefficient R^(2)=0.9998,which meets the requirements of CA chips with a milligram-level content test.Compared with the existing ICP method,component analysis results of CA chips obtained by spectrophotometry are closer to real component content in samples and have satisfactory accuracy.Moreover,as its application in miniaturized explosive systems,the ignition ability of CA chips with different component contents for direct ink writing CL-20 and the corresponding mechanism was studied.This study provided a basis and idea for the design and performance evaluation of CA chips in miniaturized explosive systems.

Characterization and ultraviolet-visible shielding property of samarium-cerium compounds containing Sm_(2)O_(2)S prepared by co-precipitation method

Since ultraviolet(UV)light,as well as blue light,which is part of visible light,is harmful to skin,samarium-cerium compounds containing Sm_(2)O_(2)S were synthesized by co-precipitation method.This kind of compounds blocks not only UV light,but also blue light.The minimum values of average transmittance(360-450 nm)and band gap of samarium-cerium compounds were 8.90%and 2.76 eV,respectively,which were less than 13.96%and 3.01 eV of CeO_(2).Elemental analysis(EA),X-ray diffraction(XRD),Fourier transformation infrared(FTIR),and Raman spectra determined that the samples contained Ce_(4)O_(7),Sm_(2)O_(2)S,Sm_(2)O_(3),and Sm_(2)O_(2)SO_(4).The microstructure of samples was analyzed by scanning and transmission electron microscopies(SEM and TEM).X-ray photoelectron spectrum(XPS)showed that cerium had Ce^(3+)and Ce^(4+) valence states,and oxygen was divided into lattice oxygen and oxygen vacancy,which was the direct cause of the decrease of average transmittance and band gap.

Analysis of Carbaryl Pesticide Residues in Environmental Samples with Spectrophotometry

A facile, rapid and sensitive spectrophotometric method was developed for the determination of carbaryl in its formulations, water and grain （rice and wheat） samples with newly synthesised reagent. The proposed method was based on the alkaline hydrolysis of carbaryl pesticide and thus resulted 1-naphthol was coupled with diazotised 4,4＇-methylene-bis-m-nitroaniline in basic medium （pH 9） to give red colored product having λmax 480 nm for diazonium method （DM） or 1-naphthol reacts with 4,4＇-methylene-bis-m-nitroaniline in the presence of oxidising agent potassium dichromate （K2Cr2O7） to give red colored product having λmax 510 nm for oxidation method （OM）. The formation of colored derivatives with the coupling agent is instantaneous and stable for 48 h （DM） and 32 h （OM） respectively. Beer＇s law was obeyed in the concentration range of 0.2--10.0 μg·mL ^-1 for DM and 0.2--0.150 μg·mL^-1 for OM. The proposed methods are sensitive, easy to operate and permitted for the determination of carbaryl with detection limits of 0.028 μg·mL^-1 for DM and 0.024 μg·mL^-1 for OM respectively. The experimental results indicate that the procedure can eliminate the fundamental interferences caused by other pesticides and non-target ions, which made the methods more sensitive and selective. The method was applicable to the determination of carbaryl residue in water and food grain samples up to μg level.

Extraction and Separation of Oxysophocarpine from Sophora alopecuroides by Reverse Three-phase Membrane Cycle Method

[Objectives] To establish the high performance liquid chromatography( HPLC) determination method for oxysophocarpine and optimize the extraction and purification technology of oxysophocarpine from Sophora alopecuroides by inverse three-phase membrane cycle.[Methods]Based on the single-factor experiment,the effects of aqueous phase and organic phase volume ratio,the concentration of sodium hydroxide,concentration of hydrochloric acid and extraction cycle time on extraction process of oxysophocarpine were investigated using orthogonal design method,to determine the optimal extraction process. [Results]The oxysophocarpine was determined by Shim-pack VP-ODS chromatographic column( 4. 6 mm × 250 mm,5 μm),mobile phase was methanol-0. 2% phosphoric acid aqueous solution( 7∶ 93),gradient elution,flow rate was 1 m L/min,the sample size was 5 μm,column temperature was 30℃,detection wavelength was 221 nm. Aqueous phase and organic phase volume ratio was 1∶ 1,hydrochloric acid concentration was 0. 3 mol/L,sodium hydroxide concentration was 0. 75 mol/L,water pump flow rate was 6 m L/min,60 min cycle time. The extraction rate of oxysophocarpine 98. 21 % within 60 min under the best experimental conditions. Oxysophocarpine has good linearity relationship within the range of 0. 01-0. 7 mg/m L( r^2= 0. 9978,n = 6),the respective average recovery rate was 97. 47%( RSD = 1. 95%). [Conclusions] This extraction process is simple in operation,the organic solvent has low consumption,and can be used for extraction of alkaloid.

Determination of Composition and Stability Constant of Praseodymium(Pr^(3+))Complex with Tribromoarsenazo(TBA)by Dual-Series Linear Regression Method

A new method,dual-series linear regression method,has been used to study the complexation equilibrium of praseodymium(Pr^(3+))with tribromoarsenazo(TBA)without knowing the accurate concentra- tion of the complexing agent TBA.In 1.2 mol/L HCl solution, Pr^(3+)reacts with TBA and forms 1:3 com- plex,the conditional stability constant(lgβ_3)of the complex determined is 15.47,and its molar absorptivity(ε_3^(630))is 1.48×10~5 L·mol^(-1)·cm^(-1).

A Highly Sensitive Kinetic Spectrophotometric System and Its Analytical Potential for Chromatographic Detection of Metal Ions

Based on the inhibitory effect of metal ions on the decolourization reaction of a dye taking place in a mixed micellar medium, a differential rate method was developed for the detection of metal ions. The present kinetic spectrophotometric system has several advantages due to introduction of the mixed micelles.

STUDY ON THE ASSAY QUALITY OF FOOD GRADE GPR BY UV—VIS METHOD

In this paper, the kind of remanent small molecules in unsaturated polyester res(?) (UP resin) , the best extractant and the best suitalbe extractive time for measuring the content of these small molecules were studied using ultraviolet- visible spectrophotometry ( UV-VIS method). According to the principle of additivity lightness absorption for mixid solution, the contents of samll molecules in several kinds of cured UP resin were measured. It is pointed out that the UV-VIS method in the assay quality of food grade GRP products is more suitable to China.

Quantitative Determination of Fluoxetine in Pharmaceuticals and Plasma Samples Using Bromatometric Method

Asensitive and simple spectrophotometric method has been developed for quantitative determination of fluoxetine using bromatometric method. The method is based on the addition of measured excess amount of bromate-bromide mixture to fluoxetine in hydrochloric acid medium. The residual bromine was determined by reacting with a fixed amount ofmethyl orange and absorbance was measured at 505 nm. The amount of bromine reacted corresponds to the amount of fluoxetine. Linear relationship between absorbance and fluoxetine concentration was found and Beer’s law was obeyed in the concentration range of 0.4 - 12 μg·mL–1. The molar absorptivity was found to be 3.8 × 104 L·mol–1·cm–1. The limit of detection and limit of quantification was calculated and found to be 0.32 μg·mL–1 and 1.0 μg·mL–1respectively. The common excipients were investigated for their interferences effect in the assay. The validity of the developed method was checked through recoveries studies and successfully applied to the determination of fluoxetine in bulk powder, pharmaceutical formulations and spiked human plasma samples. The percent recoveries were found to be in the range of 97.0% - 101.0% for pharmaceutical formulations and from 97.0% - 99.0% for spiked human plasma.

PHOTODEGRADATION OF p-NITROCHLORBENZENE(p-NCB)USING NANOMETER-SIZED ZnO PARTICLES PREPARED BY REACTIVE EVAPORATION METHOD

Photocatalytic degradations of p-nitrochlorbenzene (p-NCB) with distilled water wereinvestigated with ZnO crystals (catalyst) of 70nm in diameter under UV irradiation.The suitable experimental conditions are determined as: ZnO 0.25g, pH 7, p-NCBconcentration 30mg/L. These variables in terms of the degradation rate have beendiscussed, which was defined as the rate of the initial degradation to the final degrada-tion of p-NCB. When all of the experimental degradation rate values are plotted as afunction of irradiation time, all of the points appeared on a single line for wide range ofp-NCB degradations. On the basis of these results, it has been concluded that at lowerZnO catalyst amount, much of the light is transmitted through the slurry in the con-tainer beaker, while at higher catalyst amount, all the incident photons are observedby the slurry. Degradation rates of p-NCB were found to decrease with increasingsolution pH. It has been concluded that the maximum degradation rate values of p-NCB under principally the same experimental conditions mentioned above are 97.4%,98.8% and 95.5% at 100min respectively. The results suggest that the photocatalyticdegradation is initiated by an oxidation of the p-NCB through ZnO surface-adsorbedhydroxyl radicals. Absorption spectra are recorded using spectrophotometer before andafter UV-irradiation in the wavelength range 200-400nm at room temperature. Itis found that the variation of irradiation time over the range 20-100min resulted inchange in the form of the spectrum linear absorption and a higher maximum valuewill be obtained at longer irradiation time.

Data processing and initial results from the CE-3 Extreme Ultraviolet Camera

The Extreme Ultraviolet Camera （EUVC） onboard the Chang＇e-3 （CE-3） lander is used to observe the structure and dynamics of Earth＇s plasmasphere from the Moon. By detecting the resonance line emission of helium ions （He＋） at 30.4 nm, the EUVC images the entire plasmasphere with a time resolution of 10 min and a spatial resolution of about 0.1 Earth radius （RE） in a single frame. We first present details about the data processing from EUVC and the data acquisition in the commissioning phase, and then report some initial results, which reflect the basic features of the plas- masphere well. The photon count and emission intensity of EUVC are consistent with previous observations and models, which indicate that the EUVC works normally and can provide high quality data for future studies.

Variation Characteristics of Ultraviolet Radiation over the North China Plain

In situ measured data of broadband solar radiation （Rs） and ultraviolet （Uv） radiation were used to investigate the spa- tiotemporal variation properties of Uv radiation and the ratio of Uv radiation to Rs over the North China Plain （NCP）. Based on the analysis, an empirical model for estimating Uv radiation under all weather conditions in this region was developed. The results showed that the annual Uv radiation over the NCP ranges from 0.38-0.52 MJ m^-2 d^-1. The highest value during the study period was recorded at the Changwu site, which is located near the margin of the Loess Plateau, while the lowest value appeared at the station in Beijing. The seasonal variation pattern of the ratio of Uv radiation to Rs is similar to that of Uv radiation; namely, the highest value appears in August and then decreases gradually until the lowest value appears in November. A small increasing trend in the Uv radiation levels and the ratio of Uv radiation to Rs was observed over the NCP. The evaluation results showed that the empirical estimation model can be widely used to estimate Uv radiation under all atmospheric conditions. The relative error between the modeled and measured daily values were within ± 15%.