Chinese Journal of Pharmaceuticals

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Synthesis of Riociguat

WANG Hongbo, DENG Qianya, YUAN Bo

2016, 47(06): 675. https://doi.org/10.16522/j.cnki.cjph.2016.06.001

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2-Fluorobenzyl bromide(14) reacted with hydrazine hydrate, cyclized with sodium salt of ethyl cyanopyruvate(3) and 1,1,3,3-tetramethoxypropane, followed by a series of functional group transforming reactions yielded 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridine-3-carboximidamide hydrochloride(9′), 9′ was cyclized with phenyldiazenyl malononitrile(10), reduction of the resulting compound with Zn powder followed by carbalkoxylation and methylation yielded riociguat(1) with an overall yield of 12.4％(based on 14).

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A New Synthetic Process of Ripasudil

WANG Xiaohua, LI Zhijie, LI Zhi, ZHANG Liu

2016, 47(06): 679. https://doi.org/10.16522/j.cnki.cjph.2016.06.002

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Ripasudil was synthesized from 4-fluoroisoquinoline-5-sulfonyl chloride by coupling reaction with (S)-2-amino-N-(tert-butoxycarbonyl)-N-(3-tert-butyldimethylsilyloxypropyl)propylamine, then subjected to hydroxy deprotection with TBAF and then Mitsunobu reaction, followed by Boc deprotection with an overall yield of about 31.3％.

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Synthesis and Inhibitory Activities Against HDAC of N-Hydroxy-3- (Substituted Phenyl)-(2E)-2-Acrylamides

SUN Hui, HUANG Hao, ZHOU Weicheng

2016, 47(06): 682. https://doi.org/10.16522/j.cnki.cjph.2016.06.003

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Nine N-hydroxy-3-(substituted phenyl)-(2E)-2-acrylamide derivatives 1a～1i were synthesized from 4-bromomethyl methyl cinnamate and (S)-2-amino-N-substituted phenyl amides. The inhibition against HDAC1 of the title compounds were tested in vitro and the results showed that all the target compounds exhibited good activity.

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Improved Synthetic Process of 4-Hexylresorcinol

JIAN Jie, YANG Hui, XU Wendong, YANG Zhaoqi, SUN Pinghua

2016, 47(06): 685. https://doi.org/10.16522/j.cnki.cjph.2016.06.004

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The anthelmintic 4-hexylresorcinol was prepared from resorcinol(2) and caproic acid via Friedel- Crafts acylation and reduction. The 4-hexanoylresorcinol(3) was quantitatively yielded at constant pressure with the reaction temperature lowered from 120 ℃ to 100 ℃ while the conventional catalysts was replaced by Et2O·BF3 in acylation. The reaction time was shorten in the second reduction reaction with the cheap and recyclable reagent Raney nickel/ hydrogen instead of zinc amalgam as reducing agent. The improved process was performed at mild reaction conditions, simplified operational equipment and cheap raw materials without using special low temperature or pressure device, therefore it is very suitable for industrialized production with an overall yield about 86％(based on compound 2).

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Optimization of Protoplast Preparation and Regeneration Conditions of Acremonium chrysogenum

YANG Song, ZHAO Chunyun, OUYANG Liming, CHU Ju, ZHANG Siliang

2016, 47(06): 687. https://doi.org/10.16522/j.cnki.cjph.2016.06.005

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The influences of cell wall degrading enzymes, enzymolysis time, composition of culture media and spreading ways on protoplast preparation and regeneration of Acremonium chrysogenum were systematically examined. The morphology of hyphae was found to have significant impact on the quality of protoplast as well. The morphologies of Acremonium chrysogenum could be described as elongated hyphae, moderately swollen hyphae and highly swollen hyphae. The morphology parameters and the evolution of mycelia morphology during culture were quantitatively described by microscopic image analysis. The relationship between hyphae morphology and the protoplast quantity were studied. The optimum conditions of protoplast preparation were as follows: moderately swollen hyphae of Acremonium chrysogenum was digested by 1％ lysing enzyme for 2 h at 30 ℃, and then the protoplasts were cultured on HCM medium with double-plated inoculation method. The number of protoplast in the broth reached 2.51×108 per milliliter, and the protoplast regeneration ratio was more than 20％.

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Selection of Precursors for Producing Gibberellin Acid by Gibberella fujikuroi and Optimization of the Fermentation Process

WANG Wei, LI Jilie, SHEN Junjun, LI Zhonghai

2016, 47(06): 692. https://doi.org/10.16522/j.cnki.cjph.2016.06.006

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A Plackett-Burman design was conducted for the selection of 8 metabolites in the liquid submerged fermentation process for gibberellin acid, aimed to improve the productivity of gibberellin acid by Gibberella fujikuroi. The results showed that oxalacetate, calcium gluconate and vitamin B2 had great influence on the yield of gibberellin acid. The optimal composition of the additive amount was approached gradually through the steepest ascent experiment as oxaloacetate 0.208 6 g/L, calcium gluconate 0.048 2 g/L, and vitamin B2 0.041 0 mg/L. Under the optimal conditions, the yield of gibberellin acid was increased to 2 396 mg/L, which was 11.6％ higher than that under the addition of mevalonate alone.

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Purification of Kelimycin with Three-stage Counter Current Extraction

LIU Hui, CHEN Kui, ZHU Jiawen, YING Xiping, YANG Shengwu

2016, 47(06): 696. https://doi.org/10.16522/j.cnki.cjph.2016.06.007

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Impurities could be divided into three groups according to their polarities: strong, medium and weak polarity. They have different solubility in distinct solvents. A three-stage counter current centrifugal extraction method was used for the purification of kelimycin. The effects of scrubbing on the removal of different impurities were also investigated. The results showed that the impurities with different polarities could be reduced after the scrubbing process, however, the removal effect on the strong polar impurities was more obvious. After optimization, the conditions were determined as follows: temperature of 20 ℃, the aqueous/ester phase ratio of 1∶1.5, RCF of 74×g and the concentration of sodium dihydrogen phosphate of 1％. The removal rate for the total impurities could be over 50％, which was a 15％ increase compared with the traditional cross flow extraction process.

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Effects of Drying Technologies on the Quality of Maca (Lepidium meyenii walpers)

DAI Chunyan, LU Huizhen, CAI Lianghui, XIN Yanrong, YANG Ye,

2016, 47(06): 702. https://doi.org/10.16522/j.cnki.cjph.2016.06.008

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The process parameters such as pre-treatment process, drying time and temperature were investigated and optimized in order to improve the drying efficiency and quality of Maca. The results showed that the appearance and nutrient contents (such as soluble extract, starch, proteins and polysaccharides) of dry Maca were decreased significantly after pretreated with steaming or high temperature wind fixing process. The optimal drying process was as follows: Maca was dried at 30 ℃ for 30 h, and then the temperature was raised to 48 ℃ at the speed of 2 ℃/6 h, then raised to 55 ℃ at the speed of 1 ℃/6 h, until the moisture content of Maca was no more than 13％. The whole process totally took about 126 h. Under the above process, the color of dry Maca was bright, with less deformation, and the fold was shallow. The contents of protein, anthocyanin and polysaccharide were 6.60％, 1.42％ and 3.57％, respectively.

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Investigation on Accumulation of Dry Weight and Active Ingredients of Paris polyphylla var. yunnanensis with Different Growth Years

LIU Limin, ZHAO Zhilian, HAN Duo, LI Haifeng,

2016, 47(06): 706. https://doi.org/10.16522/j.cnki.cjph.2016.06.009

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The accumulation regularities of dry weight and active steroidal saponins, which were extracted from the rhizomes, stems and leaves of Paris polyphylla var. yunnanensis with different growth years were investigated. An HPLC method was applied to determine the active ingredients in the rhizomes, stems and leaves. A direct weighing method was used to determine the dry weight accumulation of aboveground and underground parts of Paris polyphylla var. yunnanensis. The results showed that there were significant differences in the contents of polyphyllin Ⅰ, polyphyllin Ⅱ, polyphyllin Ⅵ, polyphyllin Ⅶ and total saponins in the rhizomes, stems and leaves(P<0.01). The chemical compositions differed in different parts, and the dry weight accumulation of the aboveground and underground parts increased yearly.

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Investigation of Stability of Exenatide Solution

YANG Ming, LUAN Hansen, WANG Hao

2016, 47(06): 711. https://doi.org/10.16522/j.cnki.cjph.2016.06.010

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An HPLC method and a circular dichroism spectroscopy were adopted to investigate the effects of pH values, temperatures, carbohydrate polymers and Zn2+ on the stability of exenatide solution. The results showed that exenatide degraded in phosphate buffer (PBS) at 37 ℃ for 10 d, and the drug content decreased by 18％ at pH 4.0 and 77％ at pH 7.4. In pH 7.4 PBS stored at 25 ℃ for 10 d, the exenatide content decreased by 33％, whereas there was no obvious degradation of exenatide observed in PBS stored at 4 ℃ for 10 d. When adding trehalose or sucrose with exenatide in a 1∶ 1 ratio, or adding Zn2+ with lower concentration, the thermal denaturation temperature of exenatide increased from 72.8 ℃ to 94.9, 83.0 or 85.0 ℃. These results indicated that near-neutral pH environment or high temperature was destructive to the stability of exenatide, while adding trehalose, sucrose or Zn2+ could improve the stability.

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Preparation of Iguratimod Sustained-release Pellets

SHI Biwei, LIN Qiaoping, LI Xiaoqiang, XU Xiangyang, YIN Lifang

2016, 47(06): 717. https://doi.org/10.16522/j.cnki.cjph.2016.06.011

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The iguratimod (1) loaded cores were prepared with centrifugal granulator by powder layering technique, then the sustained-release pellets were obtained by coating with the protection layer and sustained-release layer in a bottom sprayed fluidized bed. A single factor experiment was adopted to optimize the influence factors affected the release profile of 1 from the pellets significantly, such as the ratio of microcrystalline cellulose to lactose in cores, additive concentration in core preparation, types and concentrations of pore-forming agent in sustained-release coating liquid, coating level of sustained-release layer. The pharmacokinetic parameters of 1 in rats after oral administration of the commercial tablets or self-made sustained-release pellets were calculated and compared. The main pharmacokinetic parameters of these two preparations were as follows: tmax (4.8±1.0) and (9.6±2.2)h, cmax (7 147±1 352) and (3 825± 830)ng/ml, MRT (7.6±1.3) and (12.1±2.3)h, AUC0→∞ (50 788±13 086) and (48 927±5 923)ng·h·ml-1, respectively. It indicated that the self-made pellets showed evident sustained-release characteristics. Its relative bioavailability was (87.6±11.6)％.

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Comparison of Fluorescence Properties of Three Kinds of CdTe Quantum Dots for Fluorescence Labelling of Nanodrug Delivery Systems

JIANG Liqun, GE Zhihua, WANG Tingyu

2016, 47(06): 723. https://doi.org/10.16522/j.cnki.cjph.2016.06.012

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Three kinds of CdTe quantum dots (QDs) with surface modification of L-cysteine (L-Cys), β-mercaptoethanol (β-ME) and thioglycolic acid (TGA) were synthesized respectively. The fluorescence intensities, half peak width to peak height ratios, diameters and fluorescence stabilities in phosphate buffer with different pH values of above QDs were compared to assess the suitability of these QDs for fluorescence labelling of nanodrug drug delivery systems. The results showed that L-Cys-CdTe-QDs possessed a high fluorescence intensity, but it could be sharply quenched in the buffers with pH values lower than 8.0. Although β-ME-CdTe-QDs would not be quenched in the range of pH 4—8, its fluorescence intensity was the weakest and the peak width was the largest. Among them, TGA-CdTe- QDs possessed the proper fluorescence intensity and peak width, and it would not be quenched in the range of pH 4— 8. Therefore, it could be predicted that TGA-CdTe-QDs was suitable for fluorescence labelling of nanodrug delivery systems.

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Formulation Optimization and in vitro Release of Osthole Liposomes

ZHANG Chenglong, ZHANG Ji, KANG Cong, MENG Xianyong, DONG Xiaohua

2016, 47(06): 728. https://doi.org/10.16522/j.cnki.cjph.2016.06.013

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The osthole liposomes were prepared by film-ultrasonic dispersion method. The formulation was optimized by single factor test and orthogonal design with entrapment efficiency as the index. The optimal parameters were as follows: the ratio of cholesterol to yolk lecithin was 1∶2, drug-to-lipid ratio was 3∶20, pH value of Tris buffer was 8.2 and hydration temperature was 40 ℃. The average particle size, ζ potential and entrapment efficiency of three batches of optimal liposomes were 260 nm, -28.1 mV and 88％, respectively. Compared with osthole solution, the in vitro release behavior of osthole from the liposomes demonstrated a sustained-release property.

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Determination of Pantoprazole Enantiomers in Dog Plasma by LC-MS/MS Using a Cellulose Chiral Chromatographic Column

CAO Xiaoli, ZAN Bin, CHEN Xiaoyan , ZHONG Dafang,

2016, 47(06): 732. https://doi.org/10.16522/j.cnki.cjph.2016.06.014

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A chiral LC-MS/MS method was established for the determination of pantoprazole (1) enantiomers in Beagle dog plasma and applied to the stereoselectivity pharmacokinetics in Beagle dog. d5-1 was selected as the internal standard and a Lux Cellulose-4 chiral column was used. MS was conducted under the multiple reaction monitoring mode with electrospray ionization (ESI), with the transitions of m/z 384.2→ m/z 200.0 (1) and m/z 389.1→ m/z 205.1 (d5-1). It was linear for (S)- and (R)-1 in the range of 2—4 000 ng/ml. The results for the stereoselectivity pharmacokinetics in Beagle dog showed that the pharmacokinetics was consistent for (S)- and (R)-1 in Beagle dogs whenever they were administered alone or as a racemic combination. There was no enatiomer detected in dog plasma after administration of a single component, indicating that there was no configuration transformation occurred.

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Determination of Ginkgolide B in Rats Urine and Feces by LC-MS/MS

KANG Xiuyuan, DING Cungang, LI Zhou, FANG Baihuan, GE Qinghua

2016, 47(06): 738. https://doi.org/10.16522/j.cnki.cjph.2016.06.015

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A LC-MS/MS method was established for the determination of ginkgolide B in rats urine and feces. The detection of the analyte and the internal standard (bilobalide) were conducted under negative ionization mode with an electrospray ionization (ESI) interface. A multiple reaction monitoring mode was chosen with the transitions of m/z 423.1→m/z 367.1 (ginkgolide B) and m/z 325.2→m/z 163.2 (bilobalide). It was linear in the concentration range of 1—250 μg/ml (urine) and 1.6—400.0 μg/g(feces). The method recoveries were 81.84％—113.8％(urine) and 83.50％—115.2％(feces). The intra- and inter-day RSDs were less than 9.7％(urine) and 10.4％(feces). The excretion pharmacokinetic in rats after intravenous injection of ginkgolide B was also investigated. The accumulated excretion rate of ginkgolide B in urine and feces was 54.09％ within 48 h.

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Determination of Regorafenib in Human Plasma by LC-MS/MS and Its Pharmacokinetics

PAN Jie, ZHOU Wenjia, WANG Meng, ZHU Yifang, ZHANG Quanying

2016, 47(06): 743. https://doi.org/10.16522/j.cnki.cjph.2016.06.016

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A LC-MS/MS method was established for the determination of regorafenib in human plasma, and was applied in the pharmacokinetics study in human. A Dikma C18 column was used, with the mobile phase of 2 mmol/L ammonium acetate solution (containing 0.1％ formic acid)∶methanol (35∶65). A tandem mass spectrometer was used, equipped with electrospray ionization source and in multiple reaction monitoring (MRM) mode, with transitions of m/z
483.1→m/z 269.9 (regorafenib) and m/z 494.1→m/z 393.9 (the internal standard, imatinib). It was linear for regorafenib in the range of 20—4 000 ng/ml. The intra- and inter-day RSDs were less than 15％. Six healthy male volunteers were administered a single oral dose of regorafenib (40 mg). The main pharmacokinetic parameters were as follows: cmax (2 187.6±332.5) ng/ml, t1/2 (6.7±2.6) h, AUC0→24 h (13 469.3±1 311.4) h·ng·ml-1, AUC0→∞ (15 321.5±1 531.5) h·ng·ml-1. Key Words:

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Determination of Ondansetron in Human Plasma by LC-MS/MS and Its Pharmacokinetics

LI Yan, GU Kai, ZHENG Xueyan

2016, 47(06): 747. https://doi.org/10.16522/j.cnki.cjph.2016.06.017

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A LC-MS/MS method was established for the determination of ondansetron (1) in human plasma,
and its pharmacokinetics after oral administration of 1 hydrochloride tablets to healthy volunteers was investigated.
Granisetron (2) was used as the internal standard. A Phenomenex-C18 column was used, with the mobile phase of
methanol∶10 mol/L ammonium acetate solution (45∶55). The mass spectrometry was conducted under the modes of
multiple reaction monitoring (MRM) and positive ion, with the transitions of m/z 294.1→m/z 170.2 (1) and m/z 313.4→
m/z 138.1 (2)。It was linear for 1 in the range of 0.1—80.0 ng/ml. The inter- and intra-day RSDs were less than 8.0％.
The main pharmacokinetic parameters of 1 in 18 male healthy volunteers after oral administration of 1 hydrochloride
tablets were as follows: cmax (51.3±6.5) ng/ml, tmax (1.6±0.2) h, t1/2 (4.2±0.9) h, AUC0→t (257.6±64.1) ng·h·ml-1, AUC0→∞
(268.0±70.1) ng·h·ml-1.
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Determination of Peramivir in Rat Plasma by HPLC and Its Pharmacokinetics

LIU Xiuju, DONG Weichong, GUO Penghui, ZHAO Yonghong, ZHAO Xi

2016, 47(06): 751. https://doi.org/10.16522/j.cnki.cjph.2016.06.018

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An HPLC method was established for the determination of peramivir in rat plasma, and its pharmacokinetics in rats was also investigated. A Diamonsil C18 column was used, with metronidazole as the internal standard and the mobile phase of 5 mmol/L potassium dihydrogen phosphate solution∶acetonitrile (85∶15), at the detection wavelength of 210 nm. It was linear for peramivir in the range of 2—200 μg/ml. The extraction recoveries were (72.5±2.7)％—(81.3±0.7)％, while the method recoveries for peramivir were (88.2±3.9)％—(102.1±2.8)％. The extraction recovery for metronidazole was (76.9±1.4)％. The major pharmacokinetic parameters in rats after iv idministration of peramivir 30 mg/kg were as follows: cmax (160.3±37.9)μg/ml, t1/2 (0.9±0.3)h, AUC0→t (96.6± 9.8)μg·h·ml-1, AUC0→∞ (107.6±38.4)μg·h·ml-1, CL (0.3±0.1)L·(h·kg)-1, V (0.4±0.1)L/kg.

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Evaluation on the Consistency of the Release Behavior in vitro between Pseudoephedrine/ Fexofenadine Sustained-release Capsules and Original Sustained-release Tablets

YUAN Chunping1,2, LIANG Huajuan2, LIN Bishan2, HUANG Zhangxin2*

2016, 47(06): 755. https://doi.org/10.16522/j.cnki.cjph.2016.06.019

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The consistency of the in vitro release behavior between pseudoephedrine/fexofenadine sustained-release capsules and original sustained-release tablets (Allegra-D®) was evaluated. The release behavior of pseudoephedrine/fexofenadine in the capsules and the original tablets was investigated in pH 1.0 hydrocloric acid, pH 3.0 hydrochloric acid, pH 4.5 phosphate buffer solution, pH 6.8 phosphate buffer solution, and water, under different rotation speeds (50 and 75 r/min) with different devices (paddle, paddle stirring with rotating basket, and basket), respectively. The uniformity and reproducibility on the release curves of three batches of industrial products were also investigated. The release curves of pseudoephedrine hydrochloride in the capsules were similar to that of the original tablets under the above conditions. The release curves of fexofenadine hydrochloride in the capsules were similar to that of the original tablets in pH 3.0 hydrochloric acid, pH 6.8 phosphate buffer solution and water at the speed of 75 r/min in paddle stirring with rotating basket, but not silimar under the other conditions. The uniformity and reproducibility of the industrial products met the technical requirements.

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Characterization and Uncertainty Evaluation of National Primary Certified Reference Material of Galanthamine Hydrobromide

YANG Dezhi, HU Kun, YANG Xuewei, Lü Yang,

2016, 47(06): 761. https://doi.org/10.16522/j.cnki.cjph.2016.06.020

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The methods were established for the uncertainty evaluation of a national primary certified reference material (CRM) of galanthamine hydrobromide. The purity of galanthamine hydrobromide CRM was certified by the joint certification including mass balance method and differential scanning calorimetry (DSC), and the uncertainty was carefully evaluated on the basis of Technical Norm of Primary Reference Material and related documents requirements of International Standards of the International Organization for Standardization (ISO). The purity of galanthamine hydrobromide CRM was 99.5％, and the uncertainty was 0.4％, with k=2, P=0.95.

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HPLC Fingerprints of Jiangzhining Granules

LIU Min, JIA Haihong, GAO Feimeng, Lü Tao, FAN Shuyan

2016, 47(06): 767. https://doi.org/10.16522/j.cnki.cjph.2016.06.021

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The HPLC fingerprints of Jiangzhining granules were established. A Diamonsil C18 column was used, with the mobile phase of methanol∶0.1％ phosphoric acid by gradient elution, at the detection wavelength of 286 nm. Ten batches of Jiangzhining granules were analyzed. There were 25 common peaks marked with the peak of 2,3,5,4'-tetrahydroxyl dibenzoethylene-2-O-β-D-glucoside as the reference and their assignment was completed. The similarities of these samples were all over 0.9 except one batch (0.731).

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Influence of Temperature on the Electrochemiluminescence Behavior of Matrine

LI Yanqing, LUO Ying, LI Lijun, CHENG Hao, HUANG Wenyi

2016, 47(06): 771. https://doi.org/10.16522/j.cnki.cjph.2016.06.022

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The influence of temperature on the electrochemiluminescence (ECL) behavior of Ru(bpy)3 2+- matrine system was studied on the gold electrode. The results showed that the temperature had a significant impact on ECL behavior of Ru(bpy)3 2+-matrine system. The electrochemical current was enhanced with the increase of temperature from 0 ℃ to 75 ℃, however the ECL intensity increased before 25 ℃ and then decreased. Under the optimum experimental conditions, it was linear for matrine in the range of 0.1—100 μmol/L. The recovery was 101.1％, with RSD of 1.58％.

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Determination of Parabens in Vacant Gelatin Capsules by Two-dimensional Liquid Chromatography

JIANG Wenming, SONG Dongmei, LE Jian, YE Xiaoxia, YANG Yongjian

2016, 47(06): 776. https://doi.org/10.16522/j.cnki.cjph.2016.06.023

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A two-dimensional liquid chromatography method was established for the determination of the parabens, including methylparaben (1), ethylparaben (2), propylparaben (3) and butylparaben (4) in vacant gelatin capsules. The parabens in samples were concentrated on the top of Boton C18 column before transferring to TSK Gel ODS
C18 column for separation. The 0.02 mol/L ammonium acetate solution and methanol were used as the mobile phase for gradient elution and the detection wavelength was set at 254 nm. Compounds 1—4 were separated completely. It was linear for the parabens in the range of 0.25—2.5 μg/ml. Their average recoveries were 99.9％, 99.4％, 98.8％ and 99.2％, with RSDs of 1.9％, 2.0％, 1.5％ and 2.2％, respectively.

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Determination of L-Cysteine Monohydrochloride in Edaravone Injection by HPLC with Pre-column Derivatization

NI Meiping, BIAN Wei, CHEN Ying, YANG Yani, HE Jun

2016, 47(06): 780. https://doi.org/10.16522/j.cnki.cjph.2016.06.024

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An HPLC method with pre-column derivatization was established for the determination of L-cysteine monohydrochloride in edaravone injection. 2,4-Dinitrochlorobenzene was used as the pre-column derivating agent. A Diamonsil C18 column was used, with the mobile phase of acetonitrile∶0.01 mol/L disodium hydrogen phosphate solution (adjusted to pH 8.0 with phosphoric acid)(40∶60), at the detection wavelength of 360 nm. It was linear for L-cysteine monohydrochloride in the range of 10—30 μg/ml. The average recovery was 101.3％, with RSD of 0.6％.

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Determination of Calcitriol by Quantitative Nuclear Magnetic Resonance

FEI Hao, CUI Feng, TANG Fei, SHA Wei, ZHANG Qingwen

2016, 47(06): 783. https://doi.org/10.16522/j.cnki.cjph.2016.06.025

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A quantitative nuclear magnetic resonance (QNMR) method was established for the determination of calcitriol. NMR spectra were obtained in (CD3)2CO, with maleic acid as the internal standard. The result was in compared with that obtained by HPLC external standard method which was recorded in USP 38. It showed that there was no significant difference between these two methods. A rapid and accurate QNMR method without reference standard material was established for the quantitative determination of calcitriol, which could be a reference to such kind of drug substance.

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Determination of Vitamin BT in Slimming Capsules by Capillary Electrophoresis

YU Haixia, ZHOU Hui, ZHAO Wenyan, ZHANG Hongfen, CHEN Anjia

2016, 47(06): 786. https://doi.org/10.16522/j.cnki.cjph.2016.06.026

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A capillary electrophoresis method was established for the determination of vitamin BT in slimming capsules with indirect UV detection. The method was carried out with 4 mmol/L quinine methanol solution as the absorbable matrix, 20 mmol/L sodium dihydrogen phosphate solution (pH 2.7) as the running buffer, at the operating voltage of 10 kV and the detection wavelength of 218 nm. It was linear for vitamin BT in the range of 1—40 μg/ml. The average recovery was 99.6％, with RSD of 1.9％.

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Research Progress of the Methods of Removing Palladium Residual Produced by the Palladium-Catalyzed Coupling Reaction

YIN Yuefan, HU Tao, LIU Yanlei, ZHANG Haibo

2016, 47(06): 789. https://doi.org/10.16522/j.cnki.cjph.2016.06.027

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The palladium-catalyzed coupling reaction was widely used in synthesizing active pharmaceutical ingredient (API). The more attention was paid to the issue of the palladium residual in API. This paper will summarize the methods to remove palladium residual including distillation, recrystallization, physical adsorption and complexation, and illustrate some practical applications in the pharmaceutical industry.

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Advances of Ion Exchange Resins as Drug Carriers

SUN Yandong, ZHANG Ranran, ZHAO Yuan, LU Weigen

2016, 47(06): 802. https://doi.org/10.16522/j.cnki.cjph.2016.06.028

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With the development of multidisciplinary and interdisciplinary studies, ion exchange resins have been increasingly used in the field of drug delivery. Because of the properties of both acidic and basic drugs dispersing within ion exchange resins, the drug-resin complexes (drug-resinates) have many advantages, such as masking the taste of bitter active substances, increasing the dissolution rate of poorly water-soluble drugs, enhancing the storage stability in vitro and dissolution stability in vivo. The drug-resinates with the expected release rate can be obtained through coating with sustained-release materials. So, the studies of ion exchange resins in the field of sustained- and controlled-release delivery are also increasing. The recent applications of ion exchange resins as drug carriers are discussed in this paper.

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Modifications of Graphene and the Applications in Drug Delivery and Biomedical Fileds

ZHANG Baomei, WANG Yang, ZHAI Guangxi

2016, 47(06): 807. https://doi.org/10.16522/j.cnki.cjph.2016.06.029

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Graphene possesses a two-demensional honeycomb structure and it is the thinnest material with excellent physical, mechanical, optical and electrical properties. But the nature of graphene makes it difficult to disperse in water and several commonly used organic solvents, resulting in a low cellular uptake. Besides, the cytotoxicity of graphene is high. Thus, modifications are especially important to graphene in improving dispersibility and biocompatibility. This article describes different modification methods about graphene, in vitro and in vivo toxicity and the advancements about the applications in drug delivery and biomedical fields including the construct of drug carrier or multifunctional carrier, photodynamic therapy (PDT), photothermal therapy (PTT), targeting therapy and so on.

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Graphical Synthetic Routes of Ledipasvir

ZHANG Heliang, SONG Yao, ZHANG Lingling, DAI Liyan

2016, 47(06): 814. https://doi.org/10.16522/j.cnki.cjph.2016.06.030

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Longitudinal Research on Sustainable Growth Ability of Chinese Medicine Enterprises Based On Entropy Method ——A Case of Corporations In Guangdong, Jiangsu, Zhejiang And Shandong

MENG Guangxing

2016, 47(06): 818. https://doi.org/10.16522/j.cnki.cjph.2016.06.031

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