ABSTRACT
Indole-3-carbinol(I3C),an important anticancer compound found in broccoli,has attracted considerable attention.The rapid extraction and accurate analysis of I3C in the pharmaceutical industry in broccoli is challenging as I3C is unstable at low pH and high temperature.In this study,a rapid,accurate,and low-cost ultrasound-assisted dispersive-filter extraction(UADFE)technique based on poly(deep eutectic solvent)-graphene oxide(PDES-GO)adsorbent was developed for the isolation and analysis of I3C in broccoli for the first time.PDES-GO with multiple adsorption interactions and a fast mass transfer rate was synthesized to accelerate adsorption and desorption.UADFE was developed by combining dispersive solid-phase extraction(DSPE)and filter solid-phase extraction(FSPE)to realize rapid extraction and separation.Based on the above two strategies,the proposed PDES-GO-UADFE method coupled with high-performance liquid chromatography(HPLC)allowed the rapid(15-16 min),accurate(84.3％-96.4％),and low-cost(adsorbent:3.00 mg)analysis of I3C in broccoli and was superior to solid-phase extraction,DSPE,and FSPE methods.The proposed method showed remarkable linearity(r=0.9998;range:0.0840-48.0 μg/g),low limit of quantification(0.0840 μg/g),and high precision(relative standard deviation≤5.6％).Therefore,the PDES-GO-UADFE-HPLC method shows significant potential in the field of pharmaceutical analysis for the separation and analysis of anti-cancer compounds in complex plant samples.
ABSTRACT
A rapid analysis method based on ultraviolet-visual(UV-Vis) spectroscopy, near infrared(NIR) spectroscopy and multivariable data analysis was established for quality evaluation of Shengxuebao Mixture. The contents of eight active ingredients of Shengxuebao Mixture including albiflorin, paeoniflorin, 2, 3, 5, 4'-tetra-hydroxy-stilbene-2-O-β-D-glucopyranoside, specnuezhenide,ecliptasaponin D, emodin, calycosin-7-glucoside and astragaloside Ⅳ were simultaneously detected by using this method. HPLC-UV-MS was used as a reference method for determining the contents of these ingredients. Partial least squares(PLS) analysis was implemented as a linear method for multivariate models calibrated between UV spectrum/NIR spectrum and contents of 8 ingredients. Finally, the performance of the model was evaluated by 24 batches of test samples. The results showed that both UV-Vis and NIR models gave a good calibration ability with an R~2 value above 0.9, and the prediction ability was also satisfactory, with an R~2 value higher than 0.83 for UV-Vis model and higher than 0.79 for NIR model. The overall results demonstrate that the established method is accurate, robust and fast, therefore, it can be used for rapid quality evaluation of Shengxuebao Mixture.
Subject(s)
Calibration , Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Least-Squares Analysis , Mass Spectrometry , Spectroscopy, Near-InfraredABSTRACT
Objective:To establish an HPLC method to determine vanillin in 18 dairy products. Methods:The samples were sep-arated on a C18 column (250 mm × 4. 6 mm, 5 μm) with the mobile phase of methanol and water (35∶65) at the flow rate of 1. 0 ml ·min-1 . The detection wavelength was 275 nm. Results:The LOD ( limit of detection) of vanillin was 0. 45 μg·ml-1 . Excellent linearity was obtained within the concentration range of 1.990-99.500 μg·ml-1(r=1.000 0). The average recovery of vanillin in different dairy products with low, medium and high levels varied between 96. 26% and 100. 81% with RSD of 0. 15%-2. 22%. Con-clusion:The method is simple and reproducible, which can be applied in the rapid analysis of vanillin in dairy products.
ABSTRACT
OBJECTIVE:To establish a simple and feasible method for rapid analysis of drug consumption patterns,and to im-prove the level of hospital pharmacy management. METHODS:Taking Motilium tablet as an example,the actual order amount da-ta of 24 months were analyzed by time series seasonal decomposition method;several key components of change trend were extract-ed by SPSS software,i.g. smoothed trend-cycle(STC),seasonal factors(SAF)and seasonally adjusted series(SAS). The varia-tion of components data series was observed to obtain the conclusion,and then compared with direct-vision method. RESULTS:The seasonal decomposition method had high prediction accuracy,the mean absolute percent error (MARE)(0.17) was less than that of error value by direct-vision method (0.24) significantly. CONCLUSIONS:This method can found drug consumption pat-terns quickly and accurately with the help of software. Based on this aspect,stock adjustment strategy can combine daily manage-ment and long-term dynamic management conveniently so as to improve the level of drug management.
ABSTRACT
OBJECTIVE: To establish a near infrared spectroscopy method for the determination of the concentration of tiopronin for injection. METHODS: By using optical fiber probes and 1 mm sampling accessories, the near infrared transmission reflectance spectra of tiopronin for injection from seven pharmaceutical factories were obtained. The partial least square method was applied to establish the model with HPLC as the reference method. RESULTS: The model had a good prediction performance. The value of the correlation coefficient (r2) was 99.0%, the mean difference of prediction for test sets was 1.30%, and the root mean square error of prediction (RMSEP) was 0.982%. CONCLUSION: NIR is a rapid, reliable and powerful method for the quantitation of tiopronin for injection, and can be applied to rapid drug determination on the spot and stability study. Copyright 2012 by the Chinese Pharmaceutical Association.
ABSTRACT
A rapid analysis method of piperazine ferulate tablets by optic-fiber sensing technology with UV-vis absorption spectrum was established.Qualitative and quantitative data were obtained and compared by maximum and minimum wavelength,absorbance and contrast spectra.Similarity method was used to identify authenticity of drugs.The difference of contents measured by this method and UV determination method in China Pharmacopoeia showed no statistical significance (P＞0.05),while the similarity can be used as a parameter to identify the authenticity of drugs.
ABSTRACT
Objective To explore the effeetiviness of the method of LabSOCS(Laboratory sourceless calibration software)efficiency calibration in laboratory rapid analysis for emergency monitoring of nuclear incidents.Methods The detection efficiency of three kinds of environmental samples in emergency monitoring Wag calculated bY using the LabSOCS efficiency calibration method,and compared with the values that were obtained by way of radioactive source calibration method.Results The maximum relative deviation of the detection efficiency between the two methods was less than 15%,and the values with relative deviation less than 5%accounted for 70%.Conclusions The LabSOCS efficiency calibration method might take the place of radioactive source efficiency calibration method,and meet the requirement of rapid analysis in emergency monitoring of the nuclear incidents.
ABSTRACT
Biochemical oxygen demand of 5 days (BOD 5) was a very important parameter of monitoring ofwater quality. The classical method presented some shortcomings,such as complexity, long period, requirementof high technology and not promptly reflecting the pollution levels of water body, so it was of no significance fortreatment of industrial waste water. In this paper, two rapid methods for determination of BODs, raising incubation temperature and correlative estimation method, were introduced and their advantages, such as short period and simplicity of operation were verified by experiments. Modification of classical method was of certain instructive significance for the practical application to treatment of industrial waste water and forecast of pollutionlevels of water body.
ABSTRACT
AIM:To establish a new method of rapid analysis of puerarin in Xintong Oral Liquid by acousto-optic tunable filter-nearinfrared spectroscopy. METHODS: HPLC was used as a reference method to determine puerarin content in Xintong Oral Liquid. Calibration model based on partial least squares(PLS1) algorithm was developed to correlate the spectra and the corresponding values determined by the reference methods. RESULTS: The root mean square error of prediction(RMSEP) of the model for puerarin was 0.137 1. The determination coefficient was R～2=0.984 5. The correlation coefficient of the true value and predication value from validation was r～2=0.996 4. CONCLUSION: The method is a quick, simple and low cost assay and able to be used in quantitative analysis of Xintong Oral Liquid.