Preparation technology of effective fraction of Catharsius molossus based on determination of effective composition and characterization of physico-chemical property / 中国中药杂志

<p><b>OBJECTIVE</b>To optimize the preparation technology of effective fraction of Catharsius molossus, and investigate the feasibility of process control by the physical and chemical characterization of extracts.</p><p><b>METHOD</b>Used single-factor test method, choosed the main effective components of peptides and amino acids as indexes, combined with theology, chemistry, electricity, and other characterization, the study researched the prepared technology of effective fraction of C. molossus including extraction, concentration, separation, purification, drying and so on.</p><p><b>RESULT</b>The optimal preparation technology of effective fraction of C. molossus was that soaked an amount of crude drugs with three times of 85% ethanol for 48 h, added 10 times of 85% ethanol, percolated in 4 mL x min(-1) x kg(-1), collected percolation liquid, concentrated to 1:1 at 50-55 degrees C, removed fat by frozen, adopted DA201-C macroporous resin, used 1 BV of water and 4 BV of 70% ethanol as eluting agent, collected eluant respectively. The water part was concentrated and dried, then washed twice with 85% ethanol, collected washing liquid and mixed with 70% ethanol eluant. The product was obtained by concentrating and dring. At the same time, the liquid-phase system of each link was characterized in preparation of effective fraction of C. molossus, which showed that the surface tension related to polypeptide was essentially unchanged, and the conductivity related to salt decreased by about 90% with ineffective substances closely related to salt The results showed that the preparation technology maximumly retained the effective information, and removed the invalid information.</p><p><b>CONCLUSION</b>The preparation technology of effective fraction of C. molossus is stable and reliable, and the process control in physico-chemical characterization of extracts is feasible.</p>

Simultaneous determination of peimine and peiminine in rat plasma by LC-MS/MS and its application in the pharmacokinetic study / 药学学报

To establish an LC-MS/MS method for simultaneous determination of peimine and peiminine in rat plasma after oral and intravenous administration of Fritillaria thunbergii Miq. extract, the pharmacokinetic parameters were calculated as well. Peimine, peiminine and internal standard carbamazepine were extracted from plasma with liquid-liquid extraction by ethyl acetate, then separated on a Luna C18 column by using acetonitrile-water containing 10 mmol x L(-1) ammonium formate (35:65), as mobile phase. The electrospray ionization (ESI) source was applied and operated in positive ion mode. Peimine was detected at m/z 432.4 --> 414.4, peiminine at m/z 430.4 --> 412.4 and carbamazepine (IS) at 237.1 --> 194.2. The linear calibration curves were obtained at the concentration range of 0.8-800 ng x mL(-1) for peimine and peiminine. The extraction recoveries were 94.1%-105.3% and 85.8%-98.6%, respectively. The precisions, accuracy and stability of the analytes meet the requirements. The method was shown to be effective, convenient, and suitable for simultaneous pharmacokinetic study of peimine and peiminine in rat.