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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  • 2016 Volume 47 Issue 04
    Published: 09 April 2016
      

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  • SHI Yubai, LI Cheng, MA Shaohua
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    Pterostilbene was synthesized from p-hydroxybenzaldehyde via protection into methoxymethyl ether and Wittig condensation to obtain 4-(methoxymethoxy)styrene, which was subjected to Heck cross-coupling reaction with 3,5-dimethoxybenzoyl chloride in the presence of Ru/C catalysis, and deprotection of methoxymethyl ether with an overall yield of about 78%.
  • WANG Miao, PAN Hongye, LIU Xuesong, WANG Longhu*
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    In this paper, two polymorphs of glycolide(form α, form β) were prepared. The crystal structures of two polymorphs of glycolide were all characterized by differential scanning calorimetry(DSC), infrared spectroscopy(IR), powder X-ray diffraction(PXRD) and single crystal X-ray diffraction(SCXRD). The results indicate that form α is in the orthorhombic system, space group Pbca, with unit cell parameters: a=5.245 1(6) Å, b=7.450 7(11)Å, c=11.793 4(13) Å, V=460.88(10)Å3, Z=4, while form β is in the monoclinic system, space group P121/n1, with unit cell parameters: a=6.718 1(10)Å, b=14.987 5(18)Å, c=9.647 8(17)Å, β=98.958(15)°, V=959.6(2)Å3, Z=8. Form α of glycolide are significantly different from form β in stability and moisture absorption, and the difference may influence the reactions and product quality in order to obtain polyglycolic acid.
  • XU Jun1, HUANG Zongqing1, ZHANG Xiquan2, ZHAO Wei2, FENG Jun3*
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    A vector pTAC-stb2036 was contructed and then expressed in Escherichia coli W3110 for the expression of human growth hormone variant B2036 (1). The fermentation medium and the culture conditions were optimized through single factor analysis and orthogonal design. The genetically engineered strain was cultured with 1% inoculation volume at 37 ℃, with an addition of 0.3 mmol/L IPTG to the medium at 3 h during the fermentation process, and then it was adjusted to 25 ℃ and kept on fermenting for 18 h. The yield of 1 increased to 2.8 mg/g under the optimized conditions, which increased by 8 times compared with that under the orignal conditions. The aimed protein was purified by anion-exchange and reverse phase column chromatographies with a purity over 97% and a total yield of 33.2%.
  • FENG Hua1, LIU Yingbo2*, LIU Liang2, PAN Niansong2, ZHOU Dequan3
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    An HPLC method was established for the determination of quercetin from different parts of Polygonum hydropiper L., including roots, stems, leaves, flowers and seeds, and the HPLC fingerprints were established. An Hypersil ODS2 C18 column was used, with the mobile phase of acetonitrile∶0.2% phosphoric acid (20∶80), at the detection wavelength of 360 nm. The results showed that there were great differences between the quercetin contents from different parts. It was the highest in leaves, followed by stems, flowers and seeds, and the lowest in roots. The similarities of HPLC fingerprints of the medicinal material were quite different from the parts of Polygonum hydropiper L.. The similarities were all above 0.95 for Polygonum hydropiper L. samples, but below 0.60 for different parts.
  • HUANG Yunran, LU Kewei, CHEN Ling, LIU Ying, LIANG Chaofeng*
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    This research focused on the preparation of pseudoephedrine hydrochloride sustained-release pellets by fluid-bed technology of drug layering and sustained-release coating. Then fexofenadine hydrochloride layer and the isolation layer were coated on the above sustained-release pellets in sequence to obtain the title capsules. Based on the concept of design of experiments (QbD), the critical quality attributes (CQAs) of the sustained-release pellets were optimized with Box-Behnken Design and response surface methodology(BBD-RSM). These Parameters were confirmed as weight gain of hypromellose (HPMC) layer (isolation layer), weight ratio of ethylcellulose (EC) to HPMC in the sustained-release layer and weight gain of the sustained-release layer. The results showed that the release of pseudoephedrine hydrochloride from the optimal sustained-release pellets prepared under the conditions of 2% weight
    gain of HPMC layer, EC to HPMC in a 350∶1 ratio and 17.5% weight gain of the sustained-release layer complied with the standard. The preparation process was stable and feasible. The quality of the final capsules complied with the standard as well.
  • ZHANG Chenghao, LUO Huafei, LIN Guobei, WU Yubo, WANG Hao*
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    An HPLC method was established to determine the concentration of demethyphenidate in the receive liquid. The stability and saturation solubility of demethyphenidate in media with different pH values were investigated. The results showed that the degradation rate of demethyphenidate in pH 4.5 phosphate buffer was only 0.17% within 48 h and this medium could also maintain the sink conditions based on the results of solubility test. The effects of skin species and enhancer types on in vitro permeation behavior of demethyphenidate from the patches were further investigated. The results showed that the cumulative amount of demethyphenidate were both over 70% within 9 h with SD rat skin and nude mice skin as barriers. So, Bama miniature pig skin was chosen as the barrier because of its poor permeation. With 1,3-propanediol, oleic acid, azone, polyethylene glycol 400 or N-methylpyrrolidone as a enhancer at concentration of 5%, the cumulative amount of demethyphenidate were all slightly improved (P>0.05), while menthol at the same concentration obstruct the permeation of demethyphenidate.
  • XU Yafei, CHAI Zheng, ZHAO Jingjing, LING Chunsheng*
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    The atorvastatin calcium (1) dispersible tablets were prepared by wet granulation method. The influence of calcium carbonate amount was investigated with drug content and dissolution at 30 min of 1 from the tablets stored under the conditions of 25 ℃ and relative humidity of 75% as indexes. The results showed that the tablets containing 22% calcium carbonate were rather stable and had a high dissolution rate. The amount and joining way of disintegrating agent and adhesive amount were optimized by orthogonal experiment. The optimal 1 dispersible tablets could disintegrate within 100 s, and the dissolution behavior of 1 was similar to the commercial product (Jing shu).
  • HUANG Yunran, WANG Xiaoling, XIE Zhihong, AN Suiwei, LIANG Chaofeng*
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    An HPLC method was established for the simultaneous determination of fexofenadine hydrochloride (1) and pseudoephedrine hydrochloride (2) in compound sustained-release capsules of 1 and 2 using a Hypersil C6H5 column (4.6 mm×250 mm, 5 μm) with methanol∶0.01 mol/L potassium dihydrogen phosphate (adjusted to pH 3.2 by dilute phosphoric acid ) (75∶25) as mobile phase and detection wavelength of 215 nm. Moreover, the related substances
    of 1 and 2 were also determined by HPLC. The related substances (A, C and D) of 1 were determined with a Agilent SB-phenyl column (4.6 mm×250 mm, 5 μm) with phosphate-perchlorate buffer (pH 2.0)∶acetonitrile∶triethylamine (650∶350∶3) as mobile phase at the detection wavelength of 220 nm. The related substance B of 1 was determined with a Astec CyclobondTMⅠ2000 column (4.6 mm×250 mm, 5 μm) with acetate buffer solution (pH 4.0)∶acetonitrile
    (85∶15) as mobile phase at the detection wavelength of 220 nm. The related substances of 2 were determined with a Spherisorb CN column (4.6 mm×250 mm, 5 μm) with 1.16% ammonium acetate solution∶methanol (94∶6, adjusted to pH 4.0 by acetic acid) as mobile phase at the detection wavelength of 257 nm. Through methodology investigation, the quality research was conformed to the provisions. The results of accelerated test and long-term test showed that
    the appearance, labeled amounts and release behaviors of 1 and 2 of the compound capsules from three batches had no significant changes, which indicating the product were rather stable.
  • DING Hongwei, CHEN Guoguang, REN Lili, GAO Pan
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    A GC method was established for the determination of hydroxylamine hydrochloride in risperidone by pre-column derivation with cyclohexanone. Dichloromethane was used as the extraction reagent. An Agilent HP-5 capillary column was used, with programmed temperature, at the injection port temperature of 220 ℃ and the FID temperature of 250 ℃. It was linear in the concentration range of 5.4—12.6 μg/ml. Its recovery was 100.6%, with RSD of
    3.44%.
  • ZHOU Yimeng, ZHOU Bin*
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    An HPLC method was established for the determination of valaciclovir hydrochloride and its related substances. A Phenomenex HyperClone C18 column was used, with the mobile phase of 0.01% ammonia solution (adjusted to pH 3.5 with phosphoric acid) ∶acetonitrile (70∶30) at the detection wavelength of 251 nm. Valaciclovir hydrochloride and its related substances were separated successfully. It was linear in the concentration range of 2.5 — 5 00 mg/ml. The average recovery was 99.82%, with RSD of 0.40%.
  • GUANG Feng1, YAO Chengkuan1*, LU Canju2, SU Peng1,3, CAO Liyong1
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