Optically active form of alpha-cyano-3-phenoxybenzyl (CPB) alcohol, building block of pyrethroid insecticides, was synthesized as its acetate by the combination of anion-exchange resin (D301)-catalyzed transcyanation between m-phenoxybenzaldehyde (m-PBA) and acetone cyanohydrin (AC), and lipase (from Alcaligenes sp.)-catalyzed enantioselective transesterification of the resulting cyanohydrin with vinyl acetate. Through optimizing technological conditions, the catalyzing efficiency was improved considerably compared to methods previously reported. Concentrations of CPB acetate were determined by gas chromatograph. The enantio excess (e.e.) values of CPB acetate were measured by NMR (nuclear magnetic resonance) method. Effects of solvents and temperatures on this reaction were studied. Cyclohexane was shown to be the best solvent among the three tested solvents. 55 degrees C was the optimal temperature for higher degree of conversion. External diffusion limitation was excluded by raising the rotational speed to 220 r/min. However, internal diffusion could not be ignored, since the catalyst (lipase) was an immobilized enzyme and its particle dimension was not made small enough. The reaction rate was substantially accelerated when the reactant (m-PBA) concentration was as high as 249 mmol/L, but decreased when the initial concentration of m-PBA reached to 277 mmol/L. It was also found that the catalyzing capability of recovered lipase was high enough to use several batches. Study of the mole ratio of AC to m-PBA showed that 2:1 was the best choice. The strategy of adding base catalyst D301 was found to be an important factor in improving the degree of conversion of the reaction from 20% to 80%. The highest degree of conversion of the reaction has reached up to 80%.
Alcaligenes ; enzymology ; Benzaldehydes ; chemistry ; Combinatorial Chemistry Techniques ; methods ; Lipase ; chemistry ; Nitriles ; chemistry ; Organic Chemicals ; chemistry ; Phenyl Ethers ; chemical synthesis ; Technology, Pharmaceutical ; methods

To ensure the stability of chemistry components and the convenience of operation, ultrasound method was chosen to study in this investigation. As the total common peaks area in chromatograms was set to be evaluation index, the influence on the technology caused by extraction time, ethanol concentration and liquid-to-solid ratio was studied by using single factor methodology, and the extraction technology of Paeoniae Radix Alba was optimized by using response surface methodology. The results showed that the extracting results were most affected by ethanol concentration; liquid-to-solid ratio came the second and extraction time thirdly. The optimum ultrasonic-assisted extraction conditions were as follow: the ultrasonic extraction time was 20.06 min, the ethanol concentration in solvent was 72.04%, and the liquid-to-solid ratio was 53.38 mL · g(-1), the predicted value of total common peaks area was 2.1608 x 10(8). Under the extraction conditions after optimization, the total common peaks area was 2.1422 x 10(8), and the relative deviation between the measured and predicted value was 0.86%, so the optimized extraction technology for Paeoniae Radix Alba is suitable and feasible. Besides, for the purpose of extracting more sufficiently and completely, the optimized extraction technology had more advantages than the extraction method recorded in the monogragh of Paeoniae Radix Alba in Chinese Pharmacopoeia, which will come true the assessment and utilization comprehensively.
Paeonia ; chemistry ; Technology, Pharmaceutical ; methods

OBJECTIVETo optimize the objective technical parameter for direct processing technology of fresh-cut for Paeonia Radix Alba.

METHODPeoniflorin and TGP were employed as the indexes of quality evaluation. Combining with the appearance of the slices, we investigated the influence of slice degree and thickness, drying temperature, drying time, drying method and other factors on the quality control of Paeonia Radix Alba slices. Furthermore, the key fresh-cut technology operating procedures parameter for Paeonia Radix Alba in Bozhou was established based on the semi-works production.

RESULTIt established tentatively the method for fresh-out and fresh-out after boiled of Paeonia Radix Alba as that selected fresh or beiled Paeonia Radix Alba, then divided them from different grades and put them into a roller to crash off the skin, cleaned and then dried them 9 h at 60 degrees C (water content 28% - 32%), and then moistened 2-3 h after spraying moderate water. Cut them into 1.5-2 mm decoction pieces and dried them at 60 degrees C, cooled, and sealed them in a package.

CONCLUSIONThe industrialization of processing decoction pieces with freshly cut Paeonia Radix Alba is stable shortens processing time, avoids effectively sulfur fumigation and infiltrating and soften, and keep high quality of production.

Solvents ; chemistry ; Technology, Pharmaceutical ; methods

OBJECTIVETo optimize the process for preparing genipin with enzymolyzed geniposide by an orthogonal experiment.

METHODThe optimal enzymolysis process was selected by an orthogonal experiment, with the concentration of geniposide as the index as well as enzyme quantity, pH of enzymolysis solution, enzymolysis time and enzymolysis temperature as considerations.

RESULTThe optimal hydrolysis conditions were as follow: rough genipin samples at the concentration of 40 g x L(-1) were selected and shook on a table concentrator at a speed of 100 r x min(-1), added with beta-glucosidase-geniposide 1 : 1 (weight proportion), with pH of enzymolysis solution at 4.5, hydrolyzation temperature at 50 degrees C, the conversion rate of genipin could reach 85.8%.

CONCLUSIONThe process is so stable and feasible that it can provide theoretical basis for the preparation of genipin with enzymolyzed geniposide.

Compound libraries and chemical synthesis play important roles in drug discovery and development, and efficient synthetic techniques can greatly facilitate the drug research. This review highlights the application of some efficient synthetic techniques in drug research including microwave chemistry, click chemistry, combinatorial chemistry, cascade reactions and multicomponent reactions, as well as the construction of diverse and drug-like compound libraries.
Click Chemistry ; Combinatorial Chemistry Techniques ; methods ; Drug Discovery ; methods ; Microwaves ; Pharmaceutical Preparations ; chemical synthesis

The powder modification technology was used to improve the powder properties and microstructure of Dioscoreae Rhizoma extract powder, thereby solving the problem of poor solubility of Dioscoreae Rhizoma formula granules. The influence of modifier dosage and grinding time on the solubility of Dioscoreae Rhizoma extract powder was investigated with the solubility as the evaluation index, and the optimal modification process was selected. The particle size, fluidity, specific surface area, and other powder properties of Dioscoreae Rhizoma extract powder before and after modification were compared. At the same time, the changes in the microstructure before and after modification was observed by scanning electron microscope, and the modification principle was explored by combining with multi-light scatterer. The results showed that after adding lactose for powder modification, the solubility of Dioscoreae Rhizoma extract powder was significantly improved. The volume of insoluble substance in the liquid of modified Dioscoreae Rhizoma extract powder obtained by the optimal modification process was reduced from 3.8 mL to 0 mL, and the particles obtained by dry granulation of the modified powder could be completely dissolved within 2 min after being exposed to water, without affecting the content of its indicator components adenosine and allantoin. After modification, the particle size of Dioscoreae Rhizoma extract powder decreased significantly, d_(0.9) decreased from(77.55±4.57) μm to(37.91±0.42) μm, the specific surface area and porosity increased, and the hydrophilicity improved. The main mechanism of improving the solubility of Dioscoreae Rhizoma formula granules was the destruction of the "coating membrane" structure on the surface of starch granules and the dispersion of water-soluble excipients. This study introduced powder modification technology to solve the solubility problem of Dioscoreae Rhizoma formula granules, which provided data support for the improvement of product quality and technical references for the improvement of solubility of other similar varieties.
Powders ; Solubility ; Technology, Pharmaceutical ; Technology ; Plant Extracts ; Particle Size

The strategy of pharmaceutical industry for 2002 - 2010 period” that was approved by Primer Minister mentioned to the need of build-up priority policies for businesses which have invested to researching, developing and innovating the pharmaceutical technology, encouraging the use of generic drug and medications made in Vietnam. An authority for nationwide regulating the medication price should be established as soon as possible. The Drug Management Administration should play more active role as a bridge between manufacturers, prescribers and patients. The national manufacturers should consider employing international experts to approach and learn their experiences and management models as well as acquaint with regulations in GMP. Out-state drug quality surveillance should be available
Adjuvants, Pharmaceutic ; Drug Industry ; Technology, Pharmaceutical

To determine the optimum process conditions for dry granulating technique of Qibai Pingfei granule, granule excipient type, rolling wheel speed and pressure and feeding speed were studied. Taking shaping rate at a time, moisture absorption and dissolubility as index, the type and amount of granule excipient were determined. In addition, taking shaping rate at a time as index, parameters of rolling wheel speed and pressure and feeding speed were researched through single factor test and response surface methodology. The optimum parameters were as follows: lactose as excipient, dry extract powder to excipient at 1:2, rolling wheel speed and pressure at 10.9 Hz and 6.4 MPa and feeding speed at 7.2 Hz. After validation of three batches pilot-scale production, the optimum processing parameters for dry granulating technique of Qibai Pingfei granule is reasonable and feasible, which can provide reliable basis for production.
Drugs, Chinese Herbal ; Powders ; Technology, Pharmaceutical ; methods

OBJECTIVETo apply the membrane separation process in the concentration process of Chuanxiong Chatiao granules and to lay the foundation for its industrialized application.

METHODThe type of membrane, the optimal pressure, the optimal temperature and the optimal detergent were selected by the single factor method. A comparative study was conducted between qualities of extracts from Chuanxiong Chatiao granules by new and traditional processes.

RESULTThe type of membrane was determined to be SMN-130A2350054. The optimal pressure was 1.7 MPa. The optimal temperature was 36 degrees C and the optimal detergent was 1% sodium polyphosphate. The qualities of extracts from Chuanxiong Chatiao granules by new and traditional processes showed no difference.

CONCLUSIONThe selected membrane separation process can effectively achieve concentration and save energy. The extracts from Chuanxiong Chatiao granules by the new process show no difference with traditional processes. Therefore, it provides basis for the industrialized application of Chuanxiong Chatiao granules.