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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  • 2015 Volume 46 Issue 6
    Published: 10 June 2015
      

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  • WU Tong, CHEN Gang, WANG Yuanzhong, GUO Bin, LI Qingeng*
    Abstract ( )   Knowledge map   Save
    Bimatoprost was synthesized from (-)-Corey lactone benzoate by Swern oxidation, HWE reaction with dimethyl (2-oxo-4-phenylbutyl)phosphonate to give (1S,5R,6R,7R)-6-[(E)-3-oxo-5-phenylpent-1-en-1-yl]-7- [[(phenyl)formyl]oxy]-2-oxobicyclo[3.3.0]octan-3-one, which was subjected to reduction with sodium borohydride, deprotection, reduction, Witting reaction with (4-carboxybutyl)triphenylphosphonium bromide, methylation and ammonolysis with an overall yield of about 31.7% and an HPLC purity of 99.3%.
  • LIU Qing1, WANG Jinmin2, ZHAO Guolei2, LAI Yisheng1*
    Abstract ( )   Knowledge map   Save
    Lu r a s i d o n e h y d r o c h l o r i d e wa s s y n t h e s i z e d f r om (1R, 2R)- c y c l o h e x a n e - 1 , 2 - dicarboxylic acid by chlorination, esterification, reduction, and sulfonylation to give (1R,2R)-1,2-bis(4- toluenesulfonyloxymethyl)cyclohexane, which was subjected to condensation with 3-(piperazin-1-yl)benzo[d]- isothiazole, followed by reaction with (3aR,4S,7R,7aS)-hexahydro-1H-4,7-methanoisoindole-1,3(2H)-dione and salification with hydrochloric acid. The overall yield was about 36%.
  • HUANG Kun, HE Qilong, CHU Qingsong*
    Abstract ( )   Knowledge map   Save
    To perform the quality control of drotaverine, two related substances recorded in quality specifications were prepared, and their structures were confirmed by 1H NMR and MS. These substances were 1-(3,4-diethoxybenzyl)-6,7-diethoxyisoquinoline(A) and (6,7-diethoxy-3,4-dihydroisoquinolin-1-yl)(3,4-
    diethoxyphenyl)methanone(B).
  • LIU Gang, SUN Lin, CHEN Yujing, LI Mingzhuan
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    2-Chloro-3-amino-4-methylpyridine, the intermediate of nevirapine, was synthesized from 4-methylpyridine via nitration with concentrated nitric acid and nitro migration with sodium metabisulfite to give 3-nitro- 4-methylpyridine which was subjected to reduction with palladium on carbon, chlorination with hydrogen peroxide and concentrated hydrochloric acid with an overall yield of 52% and an HPLC purity of 99.5%.
  • XU Yu, HUANG Lei, YUAN Shuai, XU Yunhui, HUA Moli*
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    The hapten, mono aconitine-3-yl glutarate (AC-GH), was synthesized by introduction of a glutaryl group to aconitine (AC). The derivative was then conjugated with bovine serum albumin (BSA) by the active ester method to form the artificial antigen (AC-GH-BSA). Eighteen molecules of AC-GH were coupled with one molecule of BSA determined by MALDI-TOF MS. Polyclonal antibody (PAbs) was produced from immunized New Zealand rabbits and could bind to AC specifically. The titer of PAbs was 1∶1 280 000.
  • ZHANG Liuhong1,2, QIAN Yuyi1,2, ZHU Huaxu1,2, GUO Liwei1,2*, YAO Weiwei2
    Abstract ( )   Knowledge map   Save
    The application of critical osmosis pressure (COP) to the research of decotions of fructification herbs in reverse osmosis process was investigated. The relationship between the decline rate of flux and osmosis pressure of decotion was analyzed with the decotions of Tribulus terrestris L., Arctium lappa L. and Crataegus pinnatifida Bge.. The results showed that there was a positive correlation between the above two factors and the value of COP was changed
    according to the kinds of the herbal decotion. The contributions of membrane resistance at the point at which the osmotic pressure of the decotion was lower than, equal to or higher than COP were drawn. The results showed that the concentration polarization was the main cause of membrane fouling. Based on the filling results of four different blocking models, the characteristics of membrane fouling in the reverse osmosis process of the three decotions were all consistent with the complete blocking model.
  • LIU Jie, YANG Yani, HE Jun*, BIAN Wei, LI Xiaoyan
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    Based on the result of pre-test, the compositions of alprostadil microemulsions were decided. The amounts of these compositions were optimized by central composite design-response surface methodology and drawing the profiles of conductivity-water content. The process parameters, such as stirring speed, temperature and time, were optimized with particle size and drug content as indexes. The results showed that the optimal microemulsions were composed of 8% Solutol HS 15, 2% lecithin, 4% medium chain triglyceride, 6% glycerol and 80% water, and were prepared at 30 ℃ with the stirring speed of 300 r/min and for 0.5 h. The mean diameters of three batches of alprostadil microemulsion prapared according to the above results were all in the range of 23 - 25 nm, and all samples demonstrated good centrifugal stability behaviors.
  • WANG Ximiao, GUO Weiying*
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    The preparation methods and formulation of the compound liposomes loaded with capecitabine (1) and oxaliplatin (2) were optimized by single factor test and orthogonal design with the entrapment efficiency as the index. The free drug was separated from the prepared liposomes by Sephadex gel microcolumn method. The concentrations of 1 and 2 were simultaneously determined by HPLC. The results showed that the optimal product could be obtained by film
    dispersion method with the drug-lipid ratio of 1∶15, weight ratios of 1 to 2 and phospholipid to cholesterol of 10∶1 and 3∶1 and phospholipid concentration of 8 g/L. The average particle diameter of the compound liposomes was 199.1 nm, and the entrapment efficiencies of 1 and 2 were 59.8% and 52.6%. The results of in vitro cytotoxicity test showed that the compound liposomes with the weight ratio of 1 to 2 of 15∶1 displayed the strongest inhibition on the proliferation of human hepatoma cells (SMMC-7721) among the liposomes with different weight ratios. Moreover, the inhibition effect was superior to that of 1 liposomes or 2 liposomes with higher dose.
  • YANG Haowei, HOU Tieqiang, CAI Yahui, LIAN Yanju, BAI Li
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    The amounts of adhesive, filling agent, disintegrant and lubricant in formulation were optimized by single factor test with the similarity between the dissolution curves of the self-made loxoprofen sodium tablets and the reference tablets (Loxonin) in pH 1.2 hydrochloric acid as the index. The optimal tablets were prepared with 45 g of 95% ethanol as adhesive, 135 g of lactose monohydrate as filling agent, 135 g of low-substituted hydroxypropyl cellulose as disintegrant and 1% of magnesium stearate as lubricant. The calculated similarity factor (f2) values were all above 58 in pH 1.2 hydrochloric acid, pH 4.5 acetate buffer, pH 6.8 phosphate buffer and water. The results showed that the dissolution profiles of the self-made tablets prepared with a laboratory scale (1 500 tablets per batch) and pilot scale (30 000 tablets per batch) were similar with that of Loxonin.
  • LI Yan1, ZHAO Ligang2*, PENG Hongfeng3, WANG Huili1, Lü Lixun2
    Abstract ( )   Knowledge map   Save
    The drug-in-adhesive patches of rotigotine with azone, oleic acid, N-methylpyrrolidone (NMP), menthol, terpineol, 2-isopropyl-5-methylcyclohexyl heptanoate (M-HEP) or (E)-2-isopropyl-5-methylcyclohexyl octadec-9-enoate (M-OA) as penetration enhancer were prepared, respectively. The in vitro permeability test was carried out with two-chamber cells and excised rat skin to investigate the effects of pressure sensitive adhesives (PSA) and enhancers on permeation behavior of the drug in patches. The results showed that the optimal patches with Duro-Tak 87-2677 as the matrix and combined enhancers of 3% M-OA and 10% NMP had a higher penetration amount and no time lag in release. The results of preliminary stability study showed that the adhesion and in vitro transdermal property of the product stored at 30 ℃ and relative humidity of 60% for 6 months had no significant changes. The penetration amounts at 24 h of the commercial patches (Neupro, 2.4 mg/10 cm2) and the self-made patches (5 mg/10 cm2) were (254.34±46.16) and(499.36±53.27)μg/cm2.
  • GU Lingling, ZHAO Yuan, YU Lifang, LU Weigen
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    The in situ single-pass perfusion method was utilized to investigate the intestinal absorption of asiatic acid tromethamine (1) in the duodenum, jejunum, ileum and colon of rats, respectively. The results showed that 1 could be absorbed in above regions of intestine. The absorption of 1 was enhanced with the increasing of its concentration, and the absorption in colon was superior to that in other three regions of intestine in low, medial and high concentration (25,
    50 and 100 μg/ml) groups (P<0.05). In terms of the group of low concentration, the P-glycoprotein inhibitor verapamil (100 μmol/L) was found to improve the drug absorption in above four regions of the rat intestine (P<0.05).
  • DONG Li1, XIE Yumin1, ZHU Di1, WANG Aimin2, ZHENG Lin1*
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    The pharmacokinetics of caffeic acid (1), 3,4-di-O-caffeoylquinic acid(2), paeoniflorin (3) and albiflorin (4) in rats were compared, after administrated alone or in combination of Herba Erigerontis with Radix Paeoniae Rubra. Rats were intravenously administrated with Herba Erigerontis extract alone or in combination with Radix Paeoniae Rubra extract. Four compounds were simultaneously determined by UPLC-MS. The pharmacokinetic parameters were calculated by DAS2.0. In combination of Herba Erigerontis with Radix Paeoniae Rubra, the MRT0→t of 1, 3 and 4 were obviously prolonged, and the t1/2 of 2, 3 and 4 as well as the AUC0→t of 2 and 4 were increased at different levels. The results showed that pharmacokinetic characteristics of the major compounds had been improved in combination of Herba Erigerontis with Radix Paeoniae Rubra. It suggested that the herbal compatibility was reasonable.
  • HOU Yulei1,2, XIE Langui1, ZHAO Xia1, SUN Huimin1*
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    A method which combined near infrared (NIR) consistency model with infrared (IR) carbonyl index was established for the identification of recycled polyethylene (PE), in order to prevent the abuse of recycled polyethylene. Hot-pressed samples were used to establish the NIR consistency model and the IR method with carbonyl index as identification index, and followed with the sample test. By means of NIR consistency model, recycled polyethylene was identified with the accuracy rate of 92%. Generally, carbonyl indexes of recycled materials were greater than that of the new materials. The combination method of NIR model and IR carbonyl index could effectively identify recycled polyethylene and decrease the possible misjudgments corroborating with each other.
  • SHAO Qi, JING Zhixin, WANG Minjuan, SUN Ningyun, ZHANG Jundong*
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    The known extract released from salbutamol sulfate aerosol valve was determined. The antioxidant 168 was determined by HPLC, while 2,4-di-tert-butylphenol, stearic acid and palmitic acid were determined by GC. It was linear for the above four extracts in the ranges of 2.00 - 19.60, 2.00 - 20.57, 2.00 - 298.76 and 2.00 - 158.95 μg/ml. Calculated according to the permitted daily exposure, the max content of the extracts was much less than the recommended limits.
  • WANG Xueping, CUI Feng, ZHENG Tai*
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    An HPLC method was established for the determination of residual acetic acid in rivaroxaban using the new mixed-mode column, Dionex Acclaim® Mixed-Mode WAX-1, with the mobile phase of acetonitrile∶0.025 mol/L potassium dihydrogen phosphate solution (50∶50), at the detection wavelength of 210 nm. The content of acetic acid was calculated by external standard method. The calibration curve was linear in the concentration range of 1 - 10 μg/ml. The average recovery was 100.6%, with RSD of 0.10%.
  • GENG Wenfei, ZHONG Weitan, DUAN Xiangdong, LOU Xin*
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    A GC method was established for the determination of decanoic acid in fermentation broth of daptomycin. A FFAP capillary column was used, with the application of flame ionization detector. Trichloromathane was used as the extraction solvent and octanoic acid was used as the internal standard. It was linear in the range of 0.001 - 20 mg/ml. The average recovery was 99.8%, with RSD of 2.6%.
  • XU Chengyin, GUO Zhiyong*
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    A full-solid-state procaine selective electrode with high sensitivity was prepared with the ionpair of procaine-sodium tetraphenylborate as the electroactive substance, based on the hydrophobicity of poly(methyl methacrylate)-poly(dimethylaminoethyl methacrylate) (PMMA-PDMA) copolymer film and the semi-conduction of poly(o-toluidine) (POT), which could inhibit ion flux of procaine effectively. The electrode showed a linear Nernst response in the range of 1×10-7 - 1×10-3 mol/L in pH 3.5 - 5.5, with a slope of 52.04 mV/pc. The low limit of detection was 7×10-8 mol/L. With good selectivity, precision and accuracy, this electrode was practicable for the analysis of procaine in pharmaceutical preparations and human serum.
  • SUN Youli, MA Jinlong*, NI Rui, SHI Jiajun, HUANG Lele
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    Bioadhesive drug delivery system (BDDS) has become a hot research point for its adhesion to a mucosa, mucus or the surface of epithelial cells, which prolongs the residence time to improve the local or systemic therapeutic effect. This paper summarizes the evaluation methods of BDDS, including measuring the bioadhesive ability in vitro and investigating the distribution and transportation in vivo. The recent advances of the applications of BDDS
    to gastrointestinal tract, oral cavity, ophthalmic, nasal, vaginal mucosa and transdermal administrations have also been reviewed to provide reference to related researches.
  • DUAN Yuwei, YU Aihua, ZHAI Guangxi*
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    Due to large fraction of voids in inner space, hollow microspheres possess special physicochemical properties of large surface area and good thermal stability etc. Hollow microspheres can load drugs through physical encapsulation or chemical bonding. The purpose of this paper is to review the preparation technologies of hollow microspheres, such as spray drying method, template method, self-assembly method and hydrothermal route. Different ways of loading drugs are also introduced. Trends and prospects of developments and applications of hollow microspheres are discussed in the end.
  • DING Jinxi, BAI Gengliang, HUANG Zehua, LIU Pengcheng, LI Wei
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  • CONG Luoluo1,2, LI Hongyao3, BAI Yuxia3, SHAO Mingli1*
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  • YI Baxian1,2, WANG Guangping3, HUO Yanfei2, CHEN Ying2, WU Xiaoming1*
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  • FAN Di
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