RESUMO
Objective:To establish a method for the determination of 4-methyl-N-(4-(pyridin-3-yl) pyrimidin-2-yl) benzene-1,3-diamine as an impurity in the preparation of imatinib mesylate. Methods: An LC-MS/MS method was used with ESI ion source con-trolled by a positive-ion mode. The MRM mode was performed with 278. 1/106. 1 as the scanning and ion-pair. Acetonitrile solution containing ammonium formate and formic acid was used with gradient elution. Results:The linear range was 1. 572~47. 160 ng/ml(r=0. 999 7). The detection limit was 0. 002 1ng and the limit of quantitation was 0. 006 8ng. The average recovery was 100. 9% with RSD of 2. 88. The results of specificity, solution stability, repeatability and durability all met the specification. Conclusion:The meth-od is sensitive, accurate and special in the determination of 4-methyl-N-(4-(pyridin-3-yl) pyrimidin-2-yl) benzene-1,3-diamine in imatinib mesylate.
RESUMO
Objective:To evaluate the tolerance and safety of Zhengbiguanjie tablets in healthy volunteers to provide the safe dose range for phase II clinical trial. Methods:Totally 36 healthy volunteers were randomly divided into five single dose groups at different doses ranging from 400 mg to 3200 mg per day and two multiple dose groups with 1600 mg and 2400 mg for continuous 7 days. The tol-erance and safety of the tablets were observed. Results: All vital signs were normal in all the volunteers in both single and multiple dose tests. Although some indicators turned into abnormal after the administration, it was not significant for clinical judgment. Neither drug combination nor serious adverse reactions were shown during the trial. However, two mild adverse events occurred and disap-peared later without any treatment. Conclusion:All the volunteers have good tolerance to Zhengbiguanjie tablets. The study proved the safety of Zhengbiguanjie tablets at single and multiple dose.
RESUMO
Purpose The aim is to investigate the rectal suppository of low molecular weight heparin（LMWH）.Methods The suppository was prepared by way of heating and fusion，the drug release property was studied with the release test in vitro and the absorption of LMWH into blood was tested by the changes of rabbits blood coagulation time. Results The drug release property in vitro followed Fick′s diffusion equation and LMWH could enter the blood through rectal medication. Conclusion The absorption from the rectum was another route of LMWH into the blood.