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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  • 2012 Volume 43 Issue 10
    Published: 10 October 2012
      

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  • SUN Min1,2, ZONG Zai-Wei1, SUN Huan-Liang1
    2012, 43(10): 810-812.
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    4-Fluoro-5-hydroxy-2-methylindole was synthesized from 2,3,4-trifluoronitrobenzene by nucleophilic aromatic substitution with ethyl acetoacetate in the presence of NaH and acid-catalyzed decarboxylation to give 1-(2,3-difluoro-6-nitrophenyl)propan-2-one, which was subjected to hydroxylation and spontaneous ring closure upon hydrogenation under HCOONH4/Pd-C with an overall yield of about 38%.
  • ZHANG Jun1, LI Xing1, SUN Li-Wen2, ZHU Jin-Tao1*
    2012, 43(10): 812-814.
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    m-Aminophenyl acetylene, the key intermediate of antitumor agent erlotinib hydrochloride, was synthesized from m-nitrobenzaldehyde by Perkin reaction, bromine addition, elimination of hydrogen bromide and decarboxylation to give (Z)-1-bromo-2-(3-nitrophenyl)ethylene, followed by reaction with NaH and reduction with Fe/HCl with an overall yield of about 45%.
  • SONG Guo-Qiang, HE Qi-Long, HUANG Xian-Feng, SHEN Li
    2012, 43(10): 815-816.
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    2-Chloro-4-(piperidin-1-ylmethyl)pyridine, the intermediate of lafutidine, was synthesized from 2-amino-4-methylpyridine by successive chlorination with CuCl/HCl and sulfuryl chloride to give 2-chloro-4-(chloromethyl)pyridine, followed by condensation with piperidine in DMF with an overall yield of about 62%.
  • WANG Li-Jun, ZHOU Bin, HU Hai-Feng*
    2012, 43(10): 817-820.
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    A strain named SIPI-5553 kept in our laboratory was used as the starting strain for the fermentation of an antifungal lipopeptide, WF16616. By UV and NTG treatment, one mutant named SIPI-H50 exhibited higher antifungal activity and its productivity of WF16616 was 510% more than that of the original stain. Under the improved fermentation process, the productivity of strain SIPI-H50 was 804 mg/L, an 86.5% increasement compared with that of the original technology.
  • TIAN Feng1, XU De-Sheng1,2, FENG Yi, ZHENG Xiang-Wei1*
    2012, 43(10): 824-826.
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    The determination, extraction and purification of resveratrol from herbal residues of Polygonum cuspidatum Sieb. et Zucc. were investigated. The extraction process was optimized by orthogonal design with the content of resveratrol as index. The resveratrol in extract was separated by macroporous adsorptive resin and chromatography and then purified by recrystallization. The optimal extraction process was as follows: the herbal residues were extracted by 90% ethanol with solid-liquid ratio of 1∶10 at 85 ℃ (reflux) for three times in 1.5, 1 and 0.5 h, respectively. The resveratrol in the extract dissolved in water was enriched by D101 macroporous adsorptive resin, followed with separation by silica column chromatography and recrystallization in acetone. The purity of final product was above 99%.
  • LIANG Chao-Feng1, NI Qing-Chun1, CHEN Tong-Kai1, AN Sui-Wei1, QIU Yu-Wen2
    2012, 43(10): 832-836.
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    The diltiazem hydrochloride microspheres with mean diameter of about 0.25 mm were prepared by fluidized-bed tangential-spraying technology with drug-loaded particles (about 0.15 mm) which were prepared with bulk powder (≤0.075 mm) by the same technique. Then the pulsatile controlled-release pellets were prepared with the above microspheres by bottom-spraying technology. The formulations of the drug-loaded particles and pellets were optimized by single-factor test and orthogonal test, respectively. The optimal preparation was as follows: the particles were prepared by tangential-spraying technology with colloidal silica as lubricant and Kollidon VA64 as adhesive, then sprayed 50% ethanol (containing bulk powder, colloidal silica and Kollidon VA64) to obtain microspheres. The microspheres were coated with the mixture of Eudragit RS100 and Eudragit L100/S100 (1∶1) of the weight ratio of 3∶1 (containing 20% triethyl citrate as plasticizer) at coating level of 70% to obtain the pellets. The pulsatile release was observed after a lag time of about 4 h. The cumulative amount at 5 h was about 20%, then the drug was released at a nearly constant rate. Finally, the drug was completely released at 24 h. The results of stability test showed that in vitro release behavior of the product stored at (40±2)℃ [relative humidity of (75±5)%] for 6 months and (30±2)℃[relative humidity of (65±5)%] for 24 months was not significantly changed.
  • TANG Wen-Xing, FU Sheng-Nan, XING Qiao, WU Chuan-Bin, HU Hai-Yan*
    2012, 43(10): 837-841.
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    Hydrophobic triacetyl-b-cyclodextrin (TA-b-CD) and hydrophilic hydroxypropyl-b-cyclodextrin (HP-b-CD) were respectively co-lyophilized with thymopentin (1). Then the sustained-release microspheres were prepared by s/o/w emulsion-solvent evaporation method with polylactic-co-glycolic acid (PLGA) as carrier material and 1 or its co-lyophilized complex as model drug. The effects of cyclodextrins on drug loading, encapsulation efficiency and burst effect of the above three kinds of 1-PLGA microspheres were compared and the mechanism of cyclodextrins to reduce the burst effect was preliminarily discussed. The results showed that the diameter, drug loading, encapsulation efficiency and burst effect (cumulative amount at 24 h) of 1-PLGA microspheres and 1-TA-b-CD-PLGA microspheres were (62.6±1.2) and (33.9±1.1) mm, (6.37±0.22)% and (8.59±0.19)%, (57.4±0.8)% and (80.4±0.6)%, 32.7% and 15.2%, respectively. However, compared with 1-PLGA microspheres, the drug loading and encapsulation efficiency of 1-HP-b-CD-PLGA microspheres were decreased and the burst effect were not significantly improved. The results of cold field scanning electron microscope, differential scanning calorimetry and powder X-ray diffraction showed that the crystal composition was changed during the co-lyophilizing process, which suggested that there had been an interaction between 1 and TA-b-CD. It might hinder the diffusion of 1 from the microspheres.
  • AN Yong-Tong1, SHEN Long-Hai1*, YIN Bei-Pei1, LIU Chang1, ZHAO Zheng-Fu2
    2012, 43(10): 842-845.
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    The A549 lung cancer-bearing nude mouse model and Lewis lung cancer-bearing mouse model were established to investigate the tumor growth inhibition of actinidin D with cyclophosphamide as positive drug. The effects of actinidin D on lymphocyte proliferation and NK cell activity of female mice bearing Lewis tumor were investigated with Polystictus glycopeptides capsules as positive drug. The results showed that compared with the saline group, actinidin D had a dose-related tumor growth inhibition on A549 and Lewis lung cancer cells in the concentration range of 150 - 600 mg/kg, while the tumor inhibitory rate of actinidin D groups was lower than that of cyclophosphamide group. The actinidin D in middle- and high-dose (300 and 600 mg/kg) group could significantly enhance lymphocyte proliferation and increase NK cell activity in Lewis cancer-bearing female mice, and this effect was superior to Polystictus glycopeptides capsules. The results suggested that actinidin D might be considered as a potent antitumor drug candidate.
  • WU Yu-Bo, ZHU Zhuang-Zhi, LUO Hua-Fei, CHEN Chun, WANG Hao*
    2012, 43(10): 849-852.
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    An UPLC-MS/MS method was established for the determination of donepezil in rat plasma with loratadine as the internal standard. The plasma samples were pretreated by liquid-liquid extraction. The mass spectrometer was used in the multiple reaction monitoring (MRM) with the ESI-positive mode. The MRM was performed at m/z 380.3→m/z 243.2 for donepezil and m/z 383.1→m/z 337.1 for loratadine. The calibration curve of donepezil was linear in the concentration range of 0.5 - 200 ng/ml. The method recoveries were between 94.1% - 106.8%. The intra- and interday RSDs were less than 10%.
  • DING Yue1, ZHANG Tong1*, TAO Jian-Sheng1, LI Meng-Yi2, CAI Zhen-Zhen1
    2012, 43(10): 857-860.
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    An HPLC method was established for the determination of plasma protein binding rates of geniposide and genipin. A C18 column was used with the mobile phase of acetonitrile-0.05% phosphoric acid(15︰85) at the detection wavelength of 238 nm. The plasma protein binding rates of geniposide and genipin with BSA, HSA and rat plasma were (38.1±4.2)% and (63.4±1.2)%, (17.6±4.9)% and (81.5±6.2)%, (24.5±3.8)% and (94.6±1.0)%, respectively. The results showed that the binding capacity of genipin with the above plasma proteins was higher than that of geniposide.
  • QIU Ying-Heng, WU Xiao-鸥, FENG Feng-Cou, PANG Xue-Bin, LI Jun
    2012, 43(10): 861-864.
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    An HPLC-DAD method was established for the determination of phenolphthalein, sibutramine and its two derivatives added illegally in slimming health care food. A C18 column was used with the mobile phase of 0.02 mol/L ammonium acetate solution (adjusted to pH 4.0 by acetic acid)-acetonitrile (56︰44) at the detection wavelength of 225 nm. The calibration curves of phenolphthalein, sibutramine and its two derivatives were linear in the range of 0.01 - 0.2 mg/ml. The recoveries were 96.8% - 103.0%, with RSDs less than 2.3%. The positive results were identified by LC-MS/MS.
  • LIU Xiao-Jun, LI Kun, BAO Yong-Chu, CHEN Qing-Hua*
    2012, 43(10): 865-870.
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    Thermosensitive biodegradable hydrogel as a novel matrix of sustained-release injectable drug delivery system has gained an increasing attention. The polyester (A) block/ polyethylene glycol (B) block triblock copolymer with good biocompatibility and biodegradation is one of the most commonly used thermosensitive polymers. The effects of some factors, including the content of polyethylene glycol block, the type of polyester block, the concentration of copolymer solution, the additive in formulation, the drug-copolymer interaction, drug loading, the shape of preparation, the pH value of medium and temperature, on the rates of copolymer degradation and drug release are reviewed in this paper. It provides useful idea and scientific basis for regulation of the rates of copolymer biodegradation and drug release in the R&D process of hydrogel injection.
  • BI Wan-Fu, DAN Xiao-Yan, SHI Hui-Lin
    2012, 43(10): 871-874.
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  • YUAN Hong-Mei, YANG Shu-Jie, SHANG Li-Yan, WU Zhi-Ang*
    2012, 43(10): 879-A92.
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