OBJECTIVETo investigate the effect of ultrasonic wave on extracting Konjac Glucomannan(KGM) in Konjac refined powder.

METHODFree reduced sugar in Konjac refined powder was removed and Konjac refined powder in the aqueous solution was processed by ultrasonic wave and KGM content was measured by spectrophotometry.

RESULTKGM content in the Konjac refined powder aqueous solution by ultrasonic process at fixed 40 kHz, 100 W, 30-45 min was equal to that by routine method at 4 h; whereas, by 1 h of ultrasonic process, KGM content was significantly enhanced than that by 4 h of routine method(P < 0.01), enhancement rate was 6.5%. Linearity of standard glucose was good (r = 0.9996) in range of 0.2-1.6 mg. The average recovery was 97.8%, RSD of repeatability was 1.27%.

CONCLUSIONUltrasonic extraction in aqueous solution is a reliable and rapid method that can enhance extraction efficiency of KGM in Konjac refined powder.

OBJECTIVETo establish the double HPLC fingerprints of water-soluble composition and amino acids precolumn derivative reagent of 13 batches of Isatidis Radix micropower.

METHODThe gradient elution was adopted with Hypersil BDS C18 column (4.6 mm x 250 mm, 5 microm). Water-soluble ingredients were detected with acetonitrile-0.1% phosphoric acid solution as mobile phase, flow rate 0.5 mL x min(-1), column temperature 20 degrees C, and the injection volume 10 microL. Amino acid ingredient were derived by PITC, and then were detected with mobile phase of 0.1 mol x L(-1) sodium acetate buffer solution (pH 6.5) - acetonitrile, flow rate 1.0 mL x min(-1), column temperature 30 degrees C, and the injection volume 5 microL. Both of the absorption wavelengths were 254 nm. Pharmacopoeia Commission "Chinese chromatographic fingerprint evaluation system (version 2.0)" was adopted to analyse, fingerprints of Isatidis Radix micropower were established, at the same time 4 main ingredients were recognized by the SPSS cluster analysis.

RESULTCommon mode of Fingerprint to water-soluble and amino acids ingredient of Isatidis Radix micropower was established, then adenosine, epigoitrin and 15 amino acids were identified as characteristic peaks. Cluster analysis showed that different kinds of the herbal Isatidis Radix micropower from different areas were different levels in the main ingredients.

CONCLUSIONDouble fingerprints of Isatidis Radix micropower is established. Each peak is optimally separated in chromatogram, which provides a scientific basis for quality control of Isatidis Radix micropower.

The quality of honeysuckle has always been an important factor in industrial development. Flowering is one of the elements for the variation of the effective components in honeysuckle. We can conveniently recognize whether the commodity is mixed with blossomed honeysuckle in the form of medicinal material. However,it is hard to identify whether the products are mixed with blossomed honeysuckle in the form of powdersince visual identification traits are missing. Therefore,this study aims to seek an effective method of odor-based distinguish for identifying the quality of honeysuckle powder in different ratios by using Heracles Ⅱ ultra-fast gas phase electronic nose.The powdered samples were prepared with flower buds and fully blooming flowers in different proportion. Gas chromatograms of the powder were obtained by HeraclesⅡ ultra-fast gas phase electronic nose. Through analyzing the data of chromatograms,we have concluded that the qualitative results of the prepared powder were almost the same,and there existed differences in the components content. Meanwhile,the hexanal odor appeared to be the critical factor in identifying honeysuckle powder quality among the flavor of all possible compounds. Also,we have applied PCA,DFA and CQ to identify and classify the variety of the powder based on the chromatogram data. Finally,it is realized that the powder was rapidly identified and classified into three grades based on the proportion of flowering honeysuckle. The predicted concentration value for the first class is less than 3,the value of is not less than 3 and less than 5 for the second class,and more than 5 for the third class. In summary,the results obtained by the study suggest that Heracles Ⅱ ultra-fast gas phase electronic nose analysis can be used as a rapid identification method for the quality of honeysuckle powder. At the same time,it can provide a reference for the quality classification of honeysuckle based on flowering degrees.
Electronic Nose ; Flowers/chemistry* ; Lonicera/chemistry* ; Odorants/analysis* ; Plant Preparations/analysis* ; Powders/analysis* ; Quality Control

We optimized the conditions of mixed fermentation of very high gravity ethanol with cassava flour and sugarcane juice. Based on the single factor experiment, we screened the important parameters for very high gravity ethanol fermentation with cassava flour and sugarcane juice by the Plackeet-burman design. Then, we obtained the optimum values of the important parameters by the orthogonal experiments: the mixing ratio of cassava flour to sugarcane juice, 1:5; initial pH of fermentation, 4.0-4.5; the concentrations of urea and MgSO4, 0.25% and 0.04% (W/W), respectively. Finally, we used a gradient temperature control strategy with the optimized conditions, and ethanol concentration of 17.84% (V/V) and fermentation efficiency of 91.82% were achieved, correspondingly.
Biofuels ; analysis ; Ethanol ; analysis ; metabolism ; Fermentation ; Hydrogen-Ion Concentration ; Manihot ; metabolism ; Powders ; Saccharum ; metabolism

AIMTo determine insulin and its related substances in insulin powder for inhalation by reversed phase high performance liquid chromatography method.

METHODSThe initial mobile phase was solution A (0.1% trifluoroacetic acid-acetonitril 70:30) and changed to solution B (0.1% trifluoroacetic acid-acetonitril 60:40) in 30 minutes. The flow rate was 2.0 mL.min-1, the column temperature was 30 degrees C, the wave length was 280 nm, the injected volume was 20 microL.

RESULTSInsulin was well separated from other peaks induced in different conditions. There was good linear relationship between the amount of insulin and its peak area, the RSD was 1.1%, the insulin solution for determination was stable in 12 hours, and the quantity detected was near the added.

CONCLUSIONThe method is simple and accurate to detect insulin and its related substances in insulin and its preparations.

The main methods of characterizing the flowability of pharmaceutical powders include repose angle method, HR method, Carr's index method, Jenike flow function method, fractal dimension method, and mass flow rate method, etc. Regarding powders with different flowabilities as the research subject, comprehensive features of pharmaceutical materials were investigated and characterized. The multivariate analysis method was employed to evaluate and analyze flowability values of the tested pharmaceutical materials. Comparing with the method of the mass flow rate, it was feasible to use multivariate analysis method to evaluate the flowability of powders. Simultaneously, the flowability of pharmaceutical materials could be ranked and definitely quantified, and critical values be determined according to the actual production, which has promoted the previous methods dependent only on the single parameter, i.e. repose angle and compression degree methods. A relatively objective standard method of evaluating flowability of powders is formed.
Multivariate Analysis ; Particle Size ; Powders ; chemistry ; Principal Component Analysis ; Technology, Pharmaceutical ; methods

OBJECTIVETo determine the content of puerarin in Xiaoke pill powder rapidly by near-infrared spectroscopy.

METHODNear-infrared diffuse reflectance spectroscopy technology was used to collect NIR spectra of Xiaoke pills powder. With HPLC analysis values as reference, the fast determination method of puerarin was established with partial least squares (PLS).

RESULTThe R2, RMSECV and RPD of the calibration model for puerarin were 0.980 1, 0.131 and 7.09. The average relative deviation of the predication set was 3.2%.

CONCLUSIONThe method is accurate, fast and simple, which could be generalized to the on-line quality control of Xiaoke pill powder production.

Percolation extraction is a conventional extraction method used in the processing of traditional Chinese medicines. After medicinal material powder is placed in a percolation tank, the extraction solvent is continuously added, and percolation extract is collected simultaneously. The percolation equipment is simple. The percolation operation is easy. It is applicable to a wide range of medicinal materials. Components that are unstable under thermal conditions can be effectively extracted. However, there are also disadvantages, such as high solvent consumption, long extraction time, and high energy consumption in subsequent concentration processes. This article mainly reviews the research progress on the common equipment types, affecting factors, parameter optimization methods, and process monitoring. According to analysis on literatures, solvent composition, impregnation time, percolation speed, and solvent consumption are considered as the important factors of percolation processes. At present, near-infrared spectroscopy is widely used in the monitoring of percolation process, and partial least square is a commonly used quantitative modeling method. According to the concept of "Quality by Design", in-depth investigation of the percolation process mechanism and development of process control methods are future development trends. Therefore, process modeling, process optimization and process monitoring shall be improved. The mechanism models and the empirical models of column chromatography can be used as references to construct the percolation process models. The effect of the quality changes of medicinal materials shall be taken into account when optimizing the percolation process parameters. More simple and easy methods shall be developed to monitor the percolation process status and key properties of percolation extracts.
Chemistry, Pharmaceutical ; Drugs, Chinese Herbal/chemistry* ; Least-Squares Analysis ; Medicine, Chinese Traditional ; Powders ; Spectroscopy, Near-Infrared

In this paper, angelica broken wall powder(ABWP) was taken as the research object, HPLC fingerprint combined with multi-component determination(ferulic acid, senkyunolide I, coniferyl ferulate, ligustilide and 3-butylidenephthalide), physical fingerprint(D_(90), particle size distribution range, particle size distribution width, bulk density, tap density, inter-particle porosity, Carr index, specific surface area, pore volume, angle of repose, Hausner ratio, loss on drying and hygroscopicity)were used to characterize the quality attribute of ABWP; similarity analysis, cluster analysis, principal component analysis and orthogonal partial least squares discriminant analysis were conducted to construct the quality evaluation method of holographic analysis based on traditional Chinese medicine QbD "4 H mode", in order to evaluate the quality of ABWP from different sources and find out differentiated indicators. The quality evaluation method could be used for scientific, comprehensive evaluation of the quality attribute of ABWP, and the quality consistency evaluation of cell-wall-broken powder of different sources or different processes.It provides new ideas for quality control and research of ultrafine granular powders of traditional Chinese medicine.
Angelica/chemistry* ; Chromatography, High Pressure Liquid ; Drugs, Chinese Herbal/analysis* ; Medicine, Chinese Traditional ; Powders ; Quality Control

In this experiment, the decoction process of famous classical formula Xiebai San was determined by optimizing the particle size of "Cuo san" and investigating the decoction process parameters, such as boiling container, water volume and duration. Xiebai San was taken as an example to explore the study method of the "Cuo san" in the famous classical formulas. The specific chromatogram of Xiebai San and the determination method of glycyrrhizin and glycyrrhizic acid in Xiebai San were established. Different particle sizes of "Cuo san" and decoction parameters were optimized based on the similarity of specific chromatogram, the specific chromatogram's peak area, the content of glycyrrhizin, the content of glycyrrhizic acid and extract yield rate.The particle size of Xiebai San powder was determined to be 2.00-4.75 mm(by four-mesh sieves). The decoction process was determined as follows: put the prescription amount into a ceramic pot, add 420 mL of water, and boil and simmer until the volume is 300 mL.The similarity of specific chromatogram was above 0.9, the specific chromatogram's peak area was larger, the content of glycyrrhizin was 0.12%, the content of glycyrrhizic acid was 0.21%,and the extract yield rate was 15.05%. The finally determined particle size of "Cuo san" can better represent the quality of Xiebai San, and is easy to prepare and suitable for industrial production.This experimental research method can comprehensively investigate the quality of Xiebai San as a whole, the content of active ingredients, and the situation of extract yield.It is a more comprehensive and objective evaluation method, and can provide experimental basis and reference for the study of other "Cuo san" famous classical formulas.
Drugs, Chinese Herbal/chemistry* ; Glycyrrhizic Acid/analysis* ; Particle Size ; Powders ; Technology, Pharmaceutical