Archive

• 
• 2012 Volume 43 Issue 1
  Published: 10 January 2012

    

  ---

• Select all
  |

• Select
  Synthesis of Solifenacin Succinate

  LI Qiang1, ZHU Jin-Lin2, HUANG Wei1, CEN Jun-Da1*

  2012, 43(1): 1-4.

  Abstract ( )   Knowledge map   Save

  Solifenacin succinate was synthesized from phenethylamine by acylation, Bischler-Napieralski cyclization, reduction by NaBH4 and resolution to afford (S)-1-phenyl-1,2,3,4-tetrahydroisoquinoline(6), which was subjected to condensation, ester exchange and then salification with an overall yield of about 21％.
• Select
  Synthesis of Prucalopride Monosuccinate

  YUAN You-Zhi, TANG Jia-Deng, CEN Jun-Da*

  2012, 43(1): 5-8.

  Abstract ( )   Knowledge map   Save

  4-Amino-5-chloro-2,3-dihydrobenzofuran-7-carboxylic acid(10) was synthesized from 4-amino- 2-hydroxybenzoic acid by esterification, acetylation,  chlorination, bromination, bromoethylation, cyclization catalysed by zinc and hydrolysis. Meanwhile 1-(3-methoxypropyl)-4-piperidine amine(11) was  synthesized from 4-piperidone hydrochloride by reaction with 3-bromopropyl methyl ether and reductive amination with ammonia in the presence of H2/Pd-C. The condensation of compounds 10 and 11 followed by salification with succinic acid to give prucalopride monosuccinate with an overall yeild of about 10％(based on 4-amino-2-hydroxybenzoic acid).
• Select
  Synthesis of Balaglitazone

  LI Ang, CHEN Guo-Hua*, ZHONG Yong-Gang

  2012, 43(1): 9-11.

  Abstract ( )   Knowledge map   Save

  Balaglitazone, an antihyperglycemic agent, was synthesized from 1H-benzo[d][1,3]oxazine-2,4- dione with methylamine to give 2-amino-N-methylbenzamide, which underwent cyclization with 2-chloroacetyl chloride, followed by etherification, Knoevenagel reaction and catalytic hydrogenation with an overall yield of about 48％.
• Select
  Synthesis of Methyl 4-Fluoro-3-methylpyridine-2-carboxylate

  SHI Qun-Feng, ZHANG Wei-Wei, ZHOU Heng, LIU Xiang-Chao, MAO Zhen-Min*

  2012, 43(1): 12-13.

  Abstract ( )   Knowledge map   Save

  Methyl 4-fluoro-3-methylpyridine-2-carboxylate (1) was synthesized from methyl 3-methylpyridine- 2-carboxylate (2) by oxidation, nitration and reduction to give methyl 4-amino-3-methylpyridine-2-carboxylate (5), followed by modified Balz-Schiemann reaction with an overall yield of about 18％ (based on compound 2).
• Select
  Synthesis of Ethyl 4-(1-Hydroxy-1-methylethyl)-2-propyl-4,5-dihydro-1H-imidazole-5-carboxylate

  WEI He-Geng1, WANG Ping2, ZHENG Guo-Jun1, LI Yi1, WU Ying-Qiu1

  2012, 43(1): 14-16.

  Abstract ( )   Knowledge map   Save

  Ethyl 4-(1-Hydroxy-1-methylethyl)-2-propyl-4,5-dihydro-1H-imidazole-5- carboxylate, a key intermediate of olmesartan medoxomil, was synthesized from 2-hydroxy-2-methylpropanenitrile by protection with trimethylsilyl, Blaise reaction, deprotection, oximation with sodium nitrite and acetic acid, reduction with Pd/C as catalyst and cyclization with methyl butanimidate hydrochloride with an overall yield of about 40％ .
• Select
  Influence Factors of Byproduct in 11α-Hydroxycanrenone Biotransformation

  ZHANG Xiao-Li, RONG Shao-Feng*, DING Bao-Mei

  2012, 43(1): 17-20.

  Abstract ( )   Knowledge map   Save

  The conditions of the byproduct formation in the 11α-hydroxycanrenone biotransformation were investigated. The byproduct was speculated to be dihydroxycanrenone by mass spectra. The single factor experiments were applied to investigate the effects of canrenone concentration, the conversion time, medium volume, rotation speed, adding substrate time and the conversion temperature on the production of byproduct. The optimal biotransformation
  conditions with lower amount of the byproduct were as follows: concentration of canrenone 6 g/L, conversion time 60 h, medium volume 100 ml/500 ml, rotation speed 160 r/min, adding substrate time at 20 h and the conversion temperature at 28 ℃ . The conversion rate of canrenone to 11α-hydroxycanrenone was 94％ .
• Select
  Screening of the Process Parameters of Ethanol Extraction of Quercetin from Euphorbia humifusa Willd. by the Combination of Artificial Neural Networks &
  Particle Swarm Optimization Algorithm

  ZHANG Ji-Xing1, WU Zhi-Nan2, CHEN Xiao-Jian2*, HE Wen3

  2012, 43(1): 21-24.

  Abstract ( )   Knowledge map   Save

  A mathematical model of relationship between the influence factors and overall desirability of evaluation indexes in the ethanol extraction of quercetin from Euphorbia humifusa Willd. was established by backpropagation (BP) artificial neural networks(ANN) . The process parameters were optimized with particle swarm optimization (PSO) algorithm. The optimal process was as follows: the quercetin was extracted with 75％ ethanol for 75 min and the ratio of ethanol to Euphorbia humifusa Willd. was 8 ∶ 1. According to the optimal process, the verification test was carried out. The results showed that the average extraction rate of quercetin was 0.11％ and the yield of dry extraction was 9.30％ (n=3). The overall desirability of evaluation indexes was better than any other results among the orthogonal design.
• Select
  Effects of Curing Conditions on Dissolution Behaviors of Film Coated Sustained Release Pellets

  XI Quan, JIN Fang*

  2012, 43(1): 25-29.

  Abstract ( )   Knowledge map   Save

  The sustained-release pellets loaded with levalbuterol hydrochloride were prepared by fluid-bed coating method with Eudragit NE30D as the coating material. The effects of different curing conditions on pellets were evaluated with in vitro release and stability of release behaviors as indexes. The results showed that both temperature and humidity contributed to the film curing process. Pellets cured under the conditions of 60 ℃ for 12 h and 60 ℃ , RH 75％
  for 6 h showed desired release profile. For both pellets, release behaviors were stable when stored under room temperature; however significant changes were observed when conditions turned harsh; under storage condition of 25 ℃ , RH 60％ , only pellets prepared by the latter treatment could remain stable.
• Select
  Effects of Lyophilization Process and Lyoprotectants on the Quality of Hydroxycamptothecine Liposomes

  DENG Li-He, WEI Min-Yan, TANG Chen-Yi, WU Chuan-Bin, XU Yue-Hong*

  2012, 43(1): 30-34.

  Abstract ( )   Knowledge map   Save

  The liposomes loaded with 10-hydroxycamptothecine were prepared by thin film hydration and high pressure homogenize method. The liposomes and free drug were separated by Sephadex G-75, the encapsulation efficiency was determined by HPLC. The eutectic points and glass transition temperatures of liposomes containing different lyoprotectants were determined by differential scanning calorimeter. The appearance, encapsulation efficiency and particle size before and after lyophilization of the products were compared to optimize the process and lyoprotectants. The results showed that 6％ sucrose was the suitable lyoprotectant, and the lyophilization process moved from prefreezing condition of 4 ℃ for 1 h，-18 ℃ for 12 h and -35 ℃ for 5 h, then lyophilized at -54 ℃ for 24 h. The lyophilized product was of good appearance, the encapsulation efficiency was (87.0±2.7)％ . The particle size varied little before and after lyophilization.
• Select
  Preparation of Carboxymethyl Chitosan Microspheres Loaded with Thymopentin for Nasal Administration and the Influence on the Ratio of CD4+/CD8+ in Rats

  SONG Qian-Qian1, WANG Xuan-Shen2, NI Ling1, BAO Qiang1, LI Fan-Zhu1*

  2012, 43(1): 35-39.

  Abstract ( )   Knowledge map   Save

  The carboxymethyl chitosan microspheres loaded with thymopentin for nasal administration were prepared by spray drying technique. The preparation was optimized by orthogonal design. The drug release behavior in vitro was determined by dialysis method. The effects of thymopentin-loaded microspheres on the ratio of CD4+/CD8+ of T-lymphocytes in immunosuppressed rats were also examined. The optimal microspheres were spherical with the mean
  diameter of (40.60±0.30)μm. The entrapment efficiency was (59.80±0.61)％ and drug loading was (15.30±0.25)％ . The in vitro release curve fitted to Higuchi equation. Compared with the negative control (saline) group, the CD4+/CD8+ ratios of high, middle and low dose (0.43, 0.30, 0.23 mg/kg) microspheres groups after nasal administration were significantly increased. There was no significant difference between high dose microspheres group and positive control (thymopentin injection, 0.1 mg/kg) group (P>0.05).
• Select
  Effects of Different Grades of PLGA on Encapsulation Efficiency and in vitro Release Behavior of Octreotide Microspheres

  YU Li, LI Min-Zhi, TONG Xin-Yong*

  2012, 43(1): 39-42.

  Abstract ( )   Knowledge map   Save

  The effects of different grades of poly(lactic acid-co-glycolic acid) (PLGA) as the carrier of watersoluble drug octreotide microspheres on drug loading, encapsulation efficiency and in vitro release behavior were investigated. The results showed that the drug loading and encapsulation efficiency decreased with the decrease of the ratio of lactide in PLGA, while the burst release increased. When the microspheres were prepared with PLGA of the same
  grade, the drug loading and encapsulation efficiency of the microspheres with higher viscosity PLGA were higher, and the burst release amount was lower. Compared with the microspheres with PLGA alone, the microspheres with the combined carrier of PLGA and poly lactic acid (PLA) had lower burst release, higher drug loading and encapsulation efficiency as well as better sustained-release behavior.
• Select
  Determination of Dissolution of Ibuprofen and Pseudoephedrine Hydrochloride Dispersible Tablets

  QIU Ying-Heng1,2, WANG Tie-Jie2, ZHOU Shou-Lin2, ZHANG Hong2, LI Qing1*

  2012, 43(1): 43-46.

  Abstract ( )   Knowledge map   Save

  The dissolubilities of ibuprofen and pseudoephedrine hydrochloride dispersible tablets in different dissolution mediums and different rotation speeds were discussed. The dissolution method was determined as follows: using the second dissolution method in Chinese Pharmacopoeia 2010 edition, at the rotation speed of 50 r/min and with the phosphate buffer solution (pH 5.5) of 900 ml. Ibuprofen and pseudoephedrine hydrochloride were detemined by
  HPLC. A C18 column was used with the mobile phase of acetonitrile-water (1︰1) (containing sodium dodecyl sulfate 2.5 g and phosphoric acid 1 ml dissolved in 1 000 ml, adjusted to pH 3.2 with ammonia) at the detection wavelength of 215 nm. The calibration curves of ibuprofen and pseudoephedrine hydrochloride were linear in the concentration ranges of 10 -1 000 μg/ml and 1.5 -150 μg/ml. The recoveries were 98.1％ and 100.4％, with RSDs of 2.6％ and 0.4％.
• Select
  Determination of Saikosaponin a and Saikosaponin d in Xiaochaihu Granules by Capillary Electrophoresis

  YI Run-Qing, SONG Fen-Yun*

  2012, 43(1): 47-50.

  Abstract ( )   Knowledge map   Save

  A capillary electrophoresis method was established for the determination of saikosaponin a and saikosaponin d in Xiaochaihu granules. An uncoated fused silica capillary column was used with benzoic acid as the internal standard and 20 mmol/L Tris + 20 mmol/L SBE-β-CD + 25 mmol/L β-CD buffer solution (pH 9.93) as the running buffer at the voltage of 12 kV. The sample was injected by gravity (10 s, 15 cm). The detection wavelength was 210 nm. Their calibration curves were linear in the concentration ranges of 10 - 100 μg/ml and 8 - 80 μg/ml. Their average recoveries were 97.1％ and 98.1％, with RSDs of 1.57％ and 1.98％.
• Select
  Determination of Montelukast in Human Plasma by LC-MS/MS

  LIU Fang1, HE Li-Juan, REN Jin-Min2, YANG Han-Yu1, ZHAO Xi1

  2012, 43(1): 50-52.

  Abstract ( )   Knowledge map   Save

  A LC-MS/MS method was established for the determination of montelukast in human plasma. A C18 column was used with the mobile phase of acetonitrile-water-formic acid (86︰14︰0.3) and simvastatin as the internal standard. Multiple reaction monitoring (MRM) mode was used with the transitions of m/z 586.3→422.5 (montelukast) and m/z 441.4→325.2 (simvastatin). The calibration curve was linear in the concentration range of 1 - 1 000 ng/ml. The recoveries were 96.7％ - 110.6％, with RSD less than 7.0％.
• Select
  Enantiomeric Separation of Terazosin by NP-HPLC

  LIU Man, ZHANG Dan, HAN Jing, LIU Hui-Chen*

  2012, 43(1): 53-56.

  Abstract ( )   Knowledge map   Save

  A NP-HPLC method was established for the enantiomeric separation of terazosin. Baseline chiral separation of terazosin enantiomers was achieved under normal-phase mode using the Chiralpak AD-H chiral column. The influences of the composition of the mobile phase, the flow rate and column temperature on the enantiomeric separation were investigated. The optimal chromatographic conditions were hexane-isopropyl alcohol-diethylamine (65︰35︰0.1)
  as the mobile phase at the flow rate of 0.7 ml/min and the detection wavelength of 254 nm at the column temperature of 25 ℃. The resolution between the peaks of terazosin enantiomers was 3.1 under the above chromatographic conditions. The calibration curves of terazosin enantiomers were linear in the concentration range of 2.5 - 7.5 μg/ml. The average recoveries were 99.8％ and 99.4％, with RSDs of 0.44％ and 0.42％.
• Select
  Quality Control for  Chuanxiong Chatiao Oral Solution

  HU Qing, JIAN Long-Hai, WANG Ke, JI Shen*

  2012, 43(1): 56-59.

  Abstract ( )   Knowledge map   Save

  Chuanxiong  Rhizoma,  Notopterygii  Rhizoma  et  Radix   and  Menthae  Haplocalycis  Herba in Chuanxiong  Chatiao oral liquid were identified by TLC, and the content of ferulic acid was determined by HPLC. The  calibration curve was linear in the range of 10 - 1 000 ng. The average recovery was about 97.7％.
• Select
  Developmental and Reproductive Toxicity Evaluation of Biopharmaceuticals

  YUAN Fang1, PAN Xiao-Liang1, LIN Hai-Xia1, WANG Qing-Li2, CHANG Yan1*

  2012, 43(1): 73-78.

  Abstract ( )   Knowledge map   Save

  Because  of  the  inherent  differences  between  small  molecule  drugs  and  large  molecule  bio-pharmaceuticals, the species specificity, immunogenicity, biological activity and exposure need to be considered for  developmental and reproductive toxicity  (DART) studies. And DART studies should take a flexible, case management,  science-based approach to research. Non-human primate models are used for DART studies when traditional species  (such as rodents and rabbit) are not pharmacologically relevant species. If biopharmaceuticals only cross-react with human and chimpanzee, the surrogate molecule, the homologous protein aimed at traditional species can be used as test substance for DART studies. In addition, transgenic animals may also be used for DART  studies.
• Select
  Improvement of  Tender Procurement of Essential Drugs System

  HAN Zhe1, GAN Rong-Fu2*

  2012, 43(1): 79-A2.

  Abstract ( )   Knowledge map   Save