主办:上海医药工业研究院
   中国药学会
   中国化学制药工业协会
ISSN 1001-8255   CN 31-1243/R   ZYGZEA

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  • 2013 Volume 44 Issue 2
    Published: 10 February 2013
      

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  • MA Yanchi1, DONG Yuanzhen1, ZHANG Xiquan2, FENG Jun1*
    2013, 44(2): 121-124.
    Abstract ( )   Knowledge map   Save
    Arg34GLP-1(7-37) was synthesized successfully from C-terminal to N-terminal according to its amino acid sequence by using Fmoc-amino acids as raw materials and Fmoc-Gly-Wang resin as a solid support. Then liraglutide was prepared by palmitoylation of the peptide chain mediated via glutamic acid. The purity of liraglutide after RP-HPLC separation was higher than 95% and the total yield was 12.8%.
  • CAI Ji-Lan, YANG Zhan-Xiong, DU You-Guo, LIU Wen-Jie
    2013, 44(2): 125-127.
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    Pelitinib, an antitumor agent, was synthesized from 2-amino-5-nitrophenol by acetylation, etherification, and reduction to give 3-ethoxy-4-acetaminoaniline, which was subjected to reaction with ethyl 2-cyano-3-ethoxyacrylate, cyclization, chlorination, deprotection and then acylation with 4-N,N-dimethylamino-2-butenoyl chloride with an overall yield of about 5%.
  • DAI Hai-Yan, HUANG Li-Qiang, WANG Xue-Qiao, ZHANG Ya-Juan, TANG Hua
    2013, 44(2): 131-133.
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    In the quality study of cefminox sodium sterile, a new impurity was identified by HPLC-MS. Its structure was speculated to be sodium (6R,7S)-7-[[[[(2S)-2-amino-2-carboxyethyl]thio]acetyl]amino]-3-[[(1-methyl-1H-tetrazol-5-yl)thio]methyl]-7-methylthio-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylate, and it was synthesized via substitution, acylation, deprotection and substitution from benzhydryl (6R,7S)-7-amino-7-methoxy-3-[(1-methyl-1H-tetrazol-5-ylthio)methyl]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylate and methanthiol. The structure was confirmed by 1H NMR and MS. It had the same peak retention time as the new impurity of cefminox sodium.
  • LI Jing-Ya, ZHOU Xing-Ning, WU Song, DU Guan-Hua, WANG Dong-Mei
    2013, 44(2): 134-137.
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    To perform the quality control of rivastigmine tartrate, eight related substances: 3-[(1S)-1-(dimethylamino-N-oxo)ethyl]phenyl ethylmethylcarbamate(3), 3-[(1S)-1-(dimethylamino)ethyl]phenol N-oxide(4), 3-vinylphenyl ethylmethylcarbamate(5), 3-acetoxylacetophenone(6), 3-acetylphenyl ethylmethylcarbamate(7), 3-[(1S)-1-(dimethylamino)ethyl]phenyl dimethylcarbamate(8), 3-[1-(dimethylamino)ethyl]phenyl ethylmethylcarbamate(9) and 3-[(1S)-1-(methylamino)ethyl]phenyl ethylmethylcarbamate(10) were synthesized. The chemical structures were confirmed by 1H NMR, 13C NMR and HRMS.
  • TENG Liang1, ZHENG Liming2, MA Guizhi 1*, LI Jian1, YU Fusheng3
    2013, 44(2): 157-161.
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    The formulation of the gastric floating tablets containing aqueous extract and microencapsulated volatile oil of Ferula sinkiangensis K.M. Shen were optimized by orthogonal design and single factor test with the in vitro release of ferulic acid as the index. The average floating onset time and duration time of the optimal formulation with 70% hydroxypropyl methyl cellulose (HPMC) K4M and 20% foaming agent (the mixture of sodium bicarbonate and citric acid with the ratio of 1∶0.76) in 0.1 mol/L HCl were (8.3±2.2)s and (22.3±2.8)h, respectively. The zero-order, Higuchi and Peppas models all fit the release data of ferulic acid well. The mechanism for controlling the drug release was polymeric erosion.
  • CHEN Dongzhi1, HONG Yang1, YANG Nan2, LI Chunxiao1, ZHANG Guangyu2*
    2013, 44(2): 162-165.
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    The ciprofloxacin chitosan microspheres for interventional bronchoscopy were prepared by phase inversion emulsification with glutaraldehyde as the crosslinking agent. The influence factors on appearance, average particle size, drug loading and encapsulation efficiency were optimized by single factor test and orthogonal design. The optimal product was spherical with the average particle size of (142.31±7.85)μm. The drug loading and encapsulation efficiency were (14.20±0.61)% and (56.43±1.31)%, respectively. The in vitro release of the product fitted to Higuchi equation. The cumulative amount at 2 h and 48 h were 44.3% and 92.1%, respectively. It indicated that the product had a sustained-release property, so that it might reduce the administration frequency.
  • HU Tianyu, LI Hua, MA Jing*
    2013, 44(2): 166-170.
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    Seventy SD rats were randomly divided into the following 5 groups: blank control, bleomycin (5 mg/kg) and oleic acid (12, 60 and 120 mg/kg) groups. All test animals were administered intranasally at a single dose. Their respiratory rate(RR), tidal volume(TV) and minute volume(MV) were recorded by computer at 0.5, 1, 2, 4 and 8 h after administration. The animals were sacrificed in three batches on d3, d7, d21. The respiratory toxicity effect of oleic acid was evaluated according to total and classified inflammatory cell count, protein concentration and lactate dehydrogenase (LDH) activity in the bronchoalveolar lavage fluid (BALF) of the left lobe of lung. The hydroxyproline (HYP) content in right upper lobe of lung was determined and the histopathologic changes of right lower lobe were
    observed. The results showed that the RR level at 0.5 h of three oleic acid groups were obviously higher than that of blank control group, while the TV level were lower. Compared with the blank control group, the total number of inflammatory cells, neutrophilic granulocyte, eosinophilic granulocytes, protein concentration and LDH activity in BALF in high dose group of oleic acid were significantly increased and lung section showed inflammatory response and numerous foam cells. There were no significant differences between three oleic acid groups and blank control group in HYP content. It indicated that high dose of oleic acid had an acute injury on rat lung tissue and affected the respiratory function, but this effect was normally reversible.
  • CHEN Shuijuan1, FU Dongjun1, GAO Shanshan1, GAO Feng1,2,3*, ZUO Jianping4
    2013, 44(2): 171-174.
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    The inclusion complexes of a water insoluble drug BMCP25 (1) with 2,6-di-O-methyl-β-cyclodextrin (DM-β-CD) were prepared by grinding method. The results of X-ray diffraction and scanning electron microscopy indicated that the drug in inclusion was changed to amorphous phase from the needle-like crystalline phase. The solubilities of 1 before and after inclusion were (0.36±0.08) and (123.82±9.81) μg/ml. An HPLC method was established for the determination of 1 in rat plasma. The pharmacokinetics of 1 in rats after iv administration (2 mg/kg) of 1 suspension or ig administration (10 mg/kg) of 1 suspension or its inclusion solution were investigated. After ig administration, the drug concentration in rat plasma was below the limit of detection in the 1 suspension group, while the oral bioavailability of 1-DM-β-CD inclusion complexes was (16.84±5.88)%. It indicated that the 1-DM-β-CD inclusion complexes could significantly enhance oral bioavailability of 1.
  • HUANG Chunyue1, YANG Yifang1*, TANG Boya1, LUO Zeyuan2, LI Cunyong2
    2013, 44(2): 175-179.
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    The chemical correlations among granules of Baitouweng decoction, its raw herbs and extracts were evaluated by HPLC fingerprint analysis. It was possible to offer a theoretical basis for the fingerprint detecting standard of granules of Baitouweng decoction. Chromatographic separation was performed on a Welch Ultimate C18 column with the mobile phase of acetonitrile-0.1% phosphoric acid (containing 0.2% triethylamine) by gradient elution at the detection wavelength of 315 nm (0 - 57 min) and 210 nm (57 - 70 min). The results showed a consistency in chemical compounds between granules of Baitouweng decoction and its raw herbs.
  • LI Limin, XIA Jing, WANG Ke, YANG Yingying, JI Shen*
    2013, 44(2): 180-185.
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    A graphite furnace atomic absorption spectrometry (GFAAS) method was established for the determination of cadmium residue in different traditional Chinese medicines (TCMs). The distribution of cadmium and its limited control measures in different TCMs were studied. The samples were digested by microwave with the optimized acid mixture, which could make all different kinds of TCMs completely digested. The 2% ammonium dihydrogen phosphate solution was selected as the matrix modifier. It was linear in the concentration range of 0 - 2 ng/ml. The recoveries of the samples with low, medium and high concentration were 81.2% - 97.4%, with RSDs less than 9%. The cadmium in 23 kinds TCMs was detected. The relative deviation between GFAAS and inductively coupled plasma-mass spectrometry (ICP-MS) was within 20%. The distribution of cadmium in different types of TCMs was as follows: animal
    medicine>leaf>whole herb>flower>rhizome>peel>fruit>root>seed.
  • ZHOU Limei1, ZENG Shaohui1, CHEN Ying2
    2013, 44(2): 185-188.
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    The anisidine values in four kinds of blank or drug-loaded fat emulsion injection were tested by the method from Chinese Pharmacopoeia Commission. The data were statistically analyzed to investigate the influence factors and the applicability of this method. The results showed that the anisidine values in fat emulsion injection, medium and long chain fat emulsion injection and propofol injection were less than 2.2 with good reproducibility, and they complied with the standard. While the anisidine value in fat-soluble vitamin injection (Ⅱ) was unreal, due to the interference of vitamins, the active ingredients in the emulsion. It seemed that determination of anisidine value in fat emulsion injection would be influenced by several factors, including sample volume, water content and different types of drug loaded in emulsion. The method was not suitable for all kinds of fat emulsion injection, so the applicability of method should be assessed.
  • ZHANG Haizhu, ZHOU Ping*, LIU Guangming, XIA Conglong, SHI Zhiting
    2013, 44(2): 189-191.
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    An HPLC method was established for the analysis and determination of the monosaccharides in polysaccharides from pinecone of Pinus armandi Franch.. The sample was hydrolyzed by trifluoroacetic acid and the hydrolysate was derivatized by reaction with 1-phenyl-3-methyl-5-pyrazolone(PMP). An Agilent Venusil XBP-C18 column was used with the mobile phase of acetonitrile-0.05 mol/L ammonium acetate buffer(pH 5.5) (20︰80) at the detection wavelength of 250 nm. The polysaccharides were composed of ten monosaccharides (including three unidentified monosaccharides). The calibration curves for the seven identified monosaccharides were linear in the range of 0.005 - 0.2 mg/ml. Their recoveries were 89.2% - 101.6%, with RSDs less than 3%. In extractions C, D, E and F from pinecone of Pinus armandi Franch., the relative average contents of mannose, rhamnose, D-glucuronic acid, D-(+) galacturonic acid, glucose, glactose and D-arabinose were 0.144% - 1.24%, 0.13% - 2.14%、0 - 0.99%, 0.17% - 2.27%, 0.76% - 2.73%, 0.14% - 9.17% and 0.16% - 8.16%, respectively.
  • ZHANG Qingwen1, YOU Qidong2, ZHOU Houyuan1*
    2013, 44(2): 192-199.
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    Molecularly targeted cancer therapy has already become one of the most important areas in cancer research. From the point view of medicinal chemistry interwoven with structural biology and translational medicine, this perspective deals with small-molecule protein kinase inhibitors launched or in late-stage clinical development focusing on drug discovery strategy, drug evolution pathway, mechanism of action, and personalized therapy paradigm.
  • XU Fenglan, LUAN Hansen*, YANG Li, WANG Hao
    2013, 44(2): 200-205.
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    The static mixers are a series of instruments for a variety of fluidic mixing depending on special structure of the internal units. The classification, geometric styles, operating principles and parameters which influence the mixing effect of different types of static mixer are introduced in this paper. In pharmaceutical field, the static mixer can be used in plenty of processes such as mixing, emulsifying, extraction and chemical reaction. It can achieve high mixing uniformity with static mixer and has the advantage of low energy consumption. However, there are also some disadvantages such as ease of blocking the pipeline, complex parameters and the lack of unified standard.
  • ZHU Yanmei, XU Danni, ZHU Xuan, CHU Shuzhen*
    2013, 44(2): 209-213.
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  • LU Ming
    2013, 44(2): 214-216.
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