A highly sensitive, rapid and rugged liquid chromatography-tandem mass spectrometw （LC-ESI-MS/MS） method was developed for reliable estimation of amantadine （AMD）, an antiviral drug in human plasma. The analyte an...A highly sensitive, rapid and rugged liquid chromatography-tandem mass spectrometw （LC-ESI-MS/MS） method was developed for reliable estimation of amantadine （AMD）, an antiviral drug in human plasma. The analyte and internal standard （IS）, amantadine-d6 （AMD-d6）, were extracted from 200μL plasma by solid phase extraction on Phenomenex Strata-X-C 33 ~t cartridges. Chromatography was performed on Synergi^TM Hydro-RP C18 （150 mm×4.6 mm, 4 μm） analytical column using a mixture of acetonitrile and 10 mM ammonium formate, pH 3.0 （80：20, v/v） as the mobile phase. Detection and quantitation was done by multiple reaction monitoring in the positive ionization mode for AMD （m/z 152.1→ 135.1 ） and IS （m/z 158.0 → 141.1） on a triple quadrupole mass spectrometer. The assay was linear in the concentration range of 0.50-500 ng/mL with correlation coefficient （r^2） 〉 0.9969. The limit of detection of the method was 0.18 ng/mL The intra-batch and inter-batch precisions were 〈 5.42% and the accuracy varied from 98.47% to 105.72%. The extraction recovery of amantadine was precise and quantitative in the range of 97.89%-100.28%. IS-normalized matrix factors for amantadine varied from 0.981 to 1.012. The stability of AMD in whole blood and plasma was evaluated under different conditions. The developed method was successfully applied for a bioequivalence study with 100 mg of AMD in 32 healthy volunteers. The reproducibility of the assay was determined by reanalysis of 134 subject samples.展开更多
A differential pulse voltammetry (DPV) method for amantadine (AT) determination is developed. To this end, all the chemical and instrumental variables affecting the determination of amantadine are optimized. These stu...A differential pulse voltammetry (DPV) method for amantadine (AT) determination is developed. To this end, all the chemical and instrumental variables affecting the determination of amantadine are optimized. These studies have used three types of glassy-carbon electrode, first electrode which has not undergone surface modification or coating, to then modify the working electrode surface with two kinds of suspensions: graphene and graphene-cucurbit[7]uril (CB[7]). From studies of the mechanisms governing the electrochemical response of amantadine, it was concluded that it is an electrochemically system with a diffusive reduction phenomenon. Under optimal conditions and with the appropriate electrode modification, we proceed to study the relation between the peak intensity with the analyte concentration. Thus, we find that when the electrode surface is covered with graphene-CB[7], two linear sections are obtained, the first one in the concentration range of between 0.05 μg·mL﹣1 and 0.75 μg·mL﹣1;and the second one between 1.00 μg·mL﹣1 and 6.00 μg·mL﹣1, with Er (%) = 87 and R.S.D. = 0.94% (n = 10 at 0.5 μg·mL﹣1 level). The minimum detectable amount was 15 ng·mL﹣1 while a concentration of 44 ng·mL﹣1 was calculated as determination limit. The optimized method was applied to the determination of amantadine in biological fluids.展开更多
Two novel polyoxometalates containing pharmaceutical component amantadine, formulated with (C10H18N) 5PMo12O40Cl2 5H2O (I) and (C10H18N) 6As2Mo18O62 6CH3CN 6H2O (II) were first synthesized and characterized by IR, UV-...Two novel polyoxometalates containing pharmaceutical component amantadine, formulated with (C10H18N) 5PMo12O40Cl2 5H2O (I) and (C10H18N) 6As2Mo18O62 6CH3CN 6H2O (II) were first synthesized and characterized by IR, UV-Vis spectra and X-ray diffraction. Structural analyses of I and II suggested that polyanions in these compounds were reserved their Keggin or Dawson structures and were linked to amantadine through electrostatic interaction and hydrogen bonding.展开更多
目的探讨不同剂量盐酸金刚烷胺对大鼠膀胱功能的影响。方法在清醒和自由活动状态下,给予成年雄性Sprague-Dawley大鼠不同剂量盐酸金刚烷胺(0.3、3、30、100μmol/kg)或安慰剂(生理盐水),连续记录(60 m in)、分析大鼠膀胱功能尿动力学参...目的探讨不同剂量盐酸金刚烷胺对大鼠膀胱功能的影响。方法在清醒和自由活动状态下,给予成年雄性Sprague-Dawley大鼠不同剂量盐酸金刚烷胺(0.3、3、30、100μmol/kg)或安慰剂(生理盐水),连续记录(60 m in)、分析大鼠膀胱功能尿动力学参数。结果安慰剂组给药后尿动力学参数没有明显变化(P>0.05);3μmol/kg盐酸金刚烷胺组大鼠给药后膀胱容量明显增加,排尿间隔时间明显延长(P<0.05);100μmol/kg盐酸金刚烷胺组大鼠给药后,膀胱容量明显减少,排尿间隔时间明显缩短(P<0.05);各剂量盐酸金刚烷胺大鼠膀胱收缩压及残余尿量均未产生明显变化(P>0.05)。结论盐酸金刚烷胺对大鼠膀胱功能具有剂量依赖性的双相作用。展开更多
文摘A highly sensitive, rapid and rugged liquid chromatography-tandem mass spectrometw （LC-ESI-MS/MS） method was developed for reliable estimation of amantadine （AMD）, an antiviral drug in human plasma. The analyte and internal standard （IS）, amantadine-d6 （AMD-d6）, were extracted from 200μL plasma by solid phase extraction on Phenomenex Strata-X-C 33 ~t cartridges. Chromatography was performed on Synergi^TM Hydro-RP C18 （150 mm×4.6 mm, 4 μm） analytical column using a mixture of acetonitrile and 10 mM ammonium formate, pH 3.0 （80：20, v/v） as the mobile phase. Detection and quantitation was done by multiple reaction monitoring in the positive ionization mode for AMD （m/z 152.1→ 135.1 ） and IS （m/z 158.0 → 141.1） on a triple quadrupole mass spectrometer. The assay was linear in the concentration range of 0.50-500 ng/mL with correlation coefficient （r^2） 〉 0.9969. The limit of detection of the method was 0.18 ng/mL The intra-batch and inter-batch precisions were 〈 5.42% and the accuracy varied from 98.47% to 105.72%. The extraction recovery of amantadine was precise and quantitative in the range of 97.89%-100.28%. IS-normalized matrix factors for amantadine varied from 0.981 to 1.012. The stability of AMD in whole blood and plasma was evaluated under different conditions. The developed method was successfully applied for a bioequivalence study with 100 mg of AMD in 32 healthy volunteers. The reproducibility of the assay was determined by reanalysis of 134 subject samples.
文摘A differential pulse voltammetry (DPV) method for amantadine (AT) determination is developed. To this end, all the chemical and instrumental variables affecting the determination of amantadine are optimized. These studies have used three types of glassy-carbon electrode, first electrode which has not undergone surface modification or coating, to then modify the working electrode surface with two kinds of suspensions: graphene and graphene-cucurbit[7]uril (CB[7]). From studies of the mechanisms governing the electrochemical response of amantadine, it was concluded that it is an electrochemically system with a diffusive reduction phenomenon. Under optimal conditions and with the appropriate electrode modification, we proceed to study the relation between the peak intensity with the analyte concentration. Thus, we find that when the electrode surface is covered with graphene-CB[7], two linear sections are obtained, the first one in the concentration range of between 0.05 μg·mL﹣1 and 0.75 μg·mL﹣1;and the second one between 1.00 μg·mL﹣1 and 6.00 μg·mL﹣1, with Er (%) = 87 and R.S.D. = 0.94% (n = 10 at 0.5 μg·mL﹣1 level). The minimum detectable amount was 15 ng·mL﹣1 while a concentration of 44 ng·mL﹣1 was calculated as determination limit. The optimized method was applied to the determination of amantadine in biological fluids.
文摘Two novel polyoxometalates containing pharmaceutical component amantadine, formulated with (C10H18N) 5PMo12O40Cl2 5H2O (I) and (C10H18N) 6As2Mo18O62 6CH3CN 6H2O (II) were first synthesized and characterized by IR, UV-Vis spectra and X-ray diffraction. Structural analyses of I and II suggested that polyanions in these compounds were reserved their Keggin or Dawson structures and were linked to amantadine through electrostatic interaction and hydrogen bonding.
文摘目的探讨不同剂量盐酸金刚烷胺对大鼠膀胱功能的影响。方法在清醒和自由活动状态下,给予成年雄性Sprague-Dawley大鼠不同剂量盐酸金刚烷胺(0.3、3、30、100μmol/kg)或安慰剂(生理盐水),连续记录(60 m in)、分析大鼠膀胱功能尿动力学参数。结果安慰剂组给药后尿动力学参数没有明显变化(P>0.05);3μmol/kg盐酸金刚烷胺组大鼠给药后膀胱容量明显增加,排尿间隔时间明显延长(P<0.05);100μmol/kg盐酸金刚烷胺组大鼠给药后,膀胱容量明显减少,排尿间隔时间明显缩短(P<0.05);各剂量盐酸金刚烷胺大鼠膀胱收缩压及残余尿量均未产生明显变化(P>0.05)。结论盐酸金刚烷胺对大鼠膀胱功能具有剂量依赖性的双相作用。
