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西安医科大学学报(英文版)
西安医科大学学报(英文版)

郑南宁

季刊

1671-8267

xyluck2003@126.com

029-82655412

710061

西安市雁塔西路76号

西安医科大学学报(英文版)/Journal Academic Journal of Xi'an Jiaotong University(English EditionCSCD
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    Separation and enrichment of trace ractopamine in biological samples by uniformly-sized molecularly imprinted polymers

    Ya LiQiang FuaMeng LiuYuan-Yuan Jiao...
    395-402页
    查看更多>>摘要：In order to prepare a high capacity packing material for solid-phase extraction with specific recognition ability of trace ractopamine in biological samples, uniformly-sized, molecularly imprinted polymers (MIPs) were prepared by a multi-step swelling and polymerization method using methacrylic acid as a functional monomer, ethylene glycol dimethacrylate as a cross-linker, and toluene as a porogen respectively. Scanning electron microscope and specific surface area were employed to identify the characteristics of MIPs. Ultraviolet spectroscopy, Fourier transform infrared spectroscopy, Scatchard analysis and kinetic study were performed to interpret the specific recognition ability and the binding process of MIPs. The results showed that, compared with other reports, MIPs synthetized in this study showed high adsorption capacity besides specific recognition ability. The adsorption capacity of MIPs was 0.063 mmol/g at 1 mmol/L ractopamine concentra- tion with the distribution coefficient 1.70. The resulting MIPs could be used as solid-phase extraction materials for separation and enrichment of trace ractopamine in biological samples.

    分子印迹聚合物莱克多巴胺生物样品Scatchard分析富集分离均匀二甲基丙烯酸酯

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    Validated LC-MS/MS method for simultaneous determination of SIM and its acid form in human plasma and cell lysate: Pharmacokinetic application

    Tamer A. AhmedJamie HornJohn HayslipMarkos Leggas...
    403-411页
    查看更多>>摘要：Simvastatin (SIM) is a 3-hydroxy-3-methylglutaryl coenzyme A reductase inhibitor widely used in hyperlipidemia therapy. SIM has recently been studied for its anticancer activity at doses higher than those used for the hyperlipidemia therapy. This prompted us to study the pharmacokinetics of high-dose SIM in cancer patients. For this purpose, an LC-MS/MS method was developed to measure SIM and its acid form (SIMA) in plasma and peripheral blood mononuclear cells (PBMCs) obtained from patients. Chromatographic analyte separation was carried out on a reverse-phase column using 75:25 (% v/v) acetonitrile:ammonium acetate (0.1 M, pH 5.0) mobile phase. Detection was performed on a triple quadrupole mass spectrometer, equipped with a turbo ion spray source and operated in positive ionization mode. The assay was linear over a range 2.5-500 ng/mL for SIM and 5-500 ng/mL for SIMA in plasma and 2.5-250 ng/mL for SIM and 5-250 ng/mL for SIMA in cell lysate. Recovery was 〉 58% for SIM and 〉 75% for SIMA in both plasma and cell lysate. SIM and SIMA were stable in plasma, cell lysate and the reconstitution solution. This method was successfully applied for the determination of SIM and SIMA in plasma and PBMCs samples collected in the pharmacokinetic study of high-dose SIM in cancer patients.

    细胞裂解液药代动力学SIM卡LC-MS同时测定人血浆MS法应用

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    Solid-state characterization fluconazol generic products and impurities determination of marketed in Morocco

    Houda BourichiYouness BrikPhilipe HubertYahia Cherrah...
    412-421页
    查看更多>>摘要：In this paper, we report the results of quality control based in pbysicochemical characteriza- tion and impurities determination of three samples of fluconazole drug substances marketed in Morocco. These samples were supplied by different pharmaceuticals companies. The sample A, as the discovered product, was supplied by Pfizer, while samples B and C (generics), were manufactured by two different Indian industries. Solid-state characterization of the three samples was realized with different physicochemical methods as: X-ray powder diffraction, Fourier-transformation infrared spectroscopy, differential scanning calorimetry. High performance liquid chromatography was used to quantify the impurities in the different samples. The results from the physicochemical methods cited above, showed difference in polymorph structure of the three drug substances. Sample A consisted in pure polymorph II1, sample B consisted in pure polymorph I1, sample C consisted in a mixture of fluconazole Form Ili, form II and the monohydrate. This result was confirmed by differential scanning calorimetry. Also it was demonstrated that solvents used during the re-crystallization step were among the origins of these differences in the structure form. On the other hand, the result of the stability study under humidity and temperature showed that fluconazole polymorphic transformation could be owed to the no compliance with the conditions of storage. The HPLC analysis of these compounds showed the presence of specific

    杂质测定产品销售氟康唑摩洛哥表征固态傅里叶变换红外光谱法差示扫描量热法

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    Chromatographic fingerprinting and quantitative analysis for the quality evaluation of Xinkeshu tablet

    Pei WangLian LiHailong YangShijuan Cheng...
    422-430页
    查看更多>>摘要：A simple, sensitive and accurate method based on high performance liquid chromato- graphy (HPLC) with diode array detector (DAD) was developed and validated for systematic quality evaluation of one type of traditional Chinese medicine preparations named Xinkeshu (XKS) tablet. In this study, the chromatographic fingerprints of XKS tablet were developed first, 23 peaks were selected as the common peaks to evaluate the similarities among different batches of XKS samples, which were manufactured in a long time span of three years. Additionally, simultaneous quantification of six markers in XKS tablet, including Danshensu, Protocatechuic aldehyde, Puerarin, Daidzin, Salvianolic acid B and Daidzein, was performed. The validation results showed that the developed method was specific, accurate, precise and robust. The preliminary explanation on why a close similarity between fingerprints did not exactly mean similar contents of chemical components in samples was given. The contribution of each chromatographic peak to similarity was also evaluated. The developed method offers an efficient, reliable and practical approach for systematic quality evaluation of XKS tablet.

    色谱指纹图谱质量评价方法定量分析二极管阵列检测器高效液相色谱法化学成分含量平板电脑相似性

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    Kinetics study of metaxalone degradation under hydrolytic, oxidative and thermal stress conditions using stability- indicating HPLC method

    Vamsi Krishna MarothuRajendra N. DashSaritha VemulaShravani Donkena...
    431-436页
    查看更多>>摘要：An isocratic stability indicating RP-HPLC-UV method is presented for the determina- tion of metaxalone (MET) in the presence of its degradation products. The method uses Dr. Maisch C18 column (250 mm × 4.6 mm, 5μm) with mobile phase consisting of acetonitrile-potassium dihydrogen orthophosphate buffer with 4 mL of 0.4% triethyl amine (pH 3.0; 10 mM) (58:42, v/v) at a flow rate of 1.0 mL/min, pH of the buffer was adjusted with o-phosphoric acid. UV detection was performed at 225 nm. The method was validated for specificity, linearity, precision, accuracy, limit of detection, limit of quantification and robustness. The calibration plot was linear over the concentration range of 1-100 μg/mL having a correlation coefficient (r2) of 0.999. Limits of detection and quantification were 0.3 and 1μg/mL, respectively. Intra-day and inter-day precision (% RSD) was 0.65 and 0.79 respectively. The proposed method was used to investigate the degradation kinetics of MET under different stress conditions employed. Degradation of MET followed a pseudo-first-order kinetics, and rate constant (K), time left for 50% potency (t1/2), and time left for 90% potency 090) were calculated.

    降解动力学HPLC方法稳定性应力条件磷酸缓冲液水解退化氧化

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    Simultaneous determination of nortriptyline hydrochloride and fluphenazine hydrochloride in microgram quantifies from low dosage forms by liquid chromatography-UV detection

    Safwan AshourNuha Kattan
    437-442页
    查看更多>>摘要：A novel method for the simultaneous high-performance liquid chromatographic determi- nation of nortriptyline hydrochloride and fluphenazine hydrochloride was developed and validated. Fhivastatin sodium was used as internal standard. The determination was performed on a Hypersil Gold Cs column (250 mm × 4.6 mm i.d., 5 μm particle size) at 25 ℃; the mobile phase, consisting of a mixture of formic acid (0.1 M, pH 2.16)-methanol (33:67, v/v), was delivered at a fow rate of 1.1 mL/min and detector wavelength at 251 rim. The retention time of nortriptyline, fluphenazine and fluvastatin was found to be 5.11, 8.05 and 11.38 min, respectively. Linearity ranges were 5.0-1350.0 and 10.0-1350.0 μg/ mL with limit of detection values of 0.72 and 0.31μg/mL, for nortriptyline and fluphenazine, respectively. Results of assay and recovery studies were statistically evaluated for its accuracy and precision. Correlation coefficients (r2) of the regression equations were greater than 0.999 in all cases. According to the validation results, the proposed method was found to be specific, accurate, precise and could be applied to the simultaneous quantitative analysis of nortriptyline and fluphenazine.

    高效液相色谱法同时测定紫外检测奋乃静盐酸低剂量氟量化

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    Cathodic adsorptive stripping voltammetry of an anti-emetic agent Granisetron in pharmaceutical formulation and biological matrix

    Rajeev JainRamkishor Sharma
    443-449页
    查看更多>>摘要：Granisetron showed one well-defined reduction peak at Hanging Mercury Drop Electrode (HMDE) in the potential range from -1.3 to -1.5 V due to reduction of C=N bond. Solid-phase extraction technique was employed for extraction of Granisetron from spiked human plasma. Granisetron showed peak current enhancement of 4.45% at square-wave voltammetry and 5.33% at cyclic voltammetry as compared with the non stripping techniques. The proposed voltammetric method allowed quantification of Granisetron in pharmaceutical formulation over the target concentration range of 5-200 ng/mL with detection limit 13.63 ng/mL, whereas in human plasma 50-225 ng/mL with detection limit 11.75 ng/mL.

    吸附溶出伏安法药物制剂生物基质固相萃取技术呕吐阴极方波伏安法循环伏安法

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    An analytical method for Fe(Ⅱ) and Fe(Ⅲ) determination in pharmaceutical grade iron sucrose complex and sodium ferric gluconate complex

    Daniele MerliAntonella ProfumoCarlo Dossi
    450-453页
    查看更多>>摘要：A robust voltammetric method has been developed and validated for the determination of Fe(Ⅱ) and Fe(Ⅲ) in pharmaceutical iron polysaccharidic complexes. Undesirable low molecular weight iron complexes, at concentration about 3% in the pharmaceutical formulation, can be easily determined with good accuracy and precision. This methodology can be proposed as a viable, environmentally sustainable substitute for the conventional Normal Pulse Polarographic method in US Pharmacopeia, with better analytical figures of merit, and reduced Hg consumption. A deeper insight in Fe(Ⅱ) and Fe(Ⅲ) composition can be gained by the combined use of a new potentiometric technique after chemical decomposition of the complex.

    葡萄糖酸亚铁Fe测定医药级蔗糖脉冲极谱法铁配合物低分子量

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    Development and validation of a simple UV spectrophotometric method for the determination of levofloxacin both in bulk and marketed dosage formulations

    Mahfuza MalequeMd. Raquibul HasanFarhad HossenSanjana Sail...
    454-457页
    查看更多>>摘要：A rapid, specific and economic UV spectrophotometric method has been developed using a solvent composed of water:methanol:acetonitrile (9:0.5:0.5) to determine the levofloxacin content in bulk and pharmaceutical dosage formulations. At a pre-determined 2 of 292 nm, it was proved linear in the range of 1.0 12.0 μg/mL, and exhibited good correlation coefficient (R2=0.9998) and excellent mean recovery (99.0-100.07%). This method was successfully applied to the determination of levofloxacin content in five marketed brands from Bangladesh and the results were in good agreement with the label claims. The method was validated statistically and by recovery studies for linearity, precision, repeatability, and reproducibility. The obtained results proved that the method can be employed for the routine analysis of levofloxacin in bulks as well as in the commercial formulations.

    分光光度法测定紫外分光光度法左氧氟沙星开发利用验证配方销售散装

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    Sensitive determination of buformin using poly-aminobenzoic acid modified glassy carbon electrode

    Gui-Ying JinHui LiWan-Bang Xu
    458-461页
    查看更多>>摘要：Glassy carbon electrode, which is used to electrochemically determine the content of buformin, is modified with an electropolymerized film of p-aminobenzoic acid in pH 7.0 acetate buffer solution (ABS). The polymer showed an excellent electrocatalytic activity for the reduction of buformin. In pH 7.0 ABS, the cathodic peak current increased linearly over three concentration intervals of buformin, and the detection limit (S/N=3) was 2.0 ×10^9 g/mL. The method was successfully applied to directly determine buformin in tablets with standard addition recoveries of 95.8 102.5%. The proposed method is simple, cheap and highly efficient.

    修饰玻碳电极氨基苯甲酸导电聚合物膜测定灵敏电催化活性加标回收率缓冲溶液

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