HPLC-ELSD法测定小儿胃安片中盐酸赖氨酸的含量

目的建立小儿胃安片中盐酸赖氨酸的含量测定方法。方法应用高效液相色谱-蒸发光散射检测仪,DiomonsilC18(250mm×4.6mm,5μm)色谱柱,以乙腈-甲醇-0.1%三氟醋酸溶液(2:1:97)为流动相,流速为0.2ml/min,测定小儿胃安片中盐酸赖氨酸的含量。结果在0.2496￣4.992μg范围内,色谱峰面积对数与对照品量的对数呈良好的线性关系r,=0.9998;平均回收率为98.02%(RSD=1.05%,n=6)。结论该法快速、简便、重现性好,可用于小儿胃安片中盐酸赖氨酸的质量控制。     

HPLC法测定复方茶碱麻黄碱片中可可碱、盐酸麻黄碱、茶碱和咖啡因的含量

建立HPLC法测定复方茶碱麻黄碱片中可可碱、盐酸麻黄碱、茶碱和咖啡因的含量。采用D iamonsil C18色谱柱,以0.05mol.L-1磷酸二氢钾-甲醇-三乙胺(77∶23∶0.2)为流动相,检测波长为215nm。线性范围为可可碱:0.1011~0.9097μg(r=0.9998);盐酸麻黄碱:0.0418~0.3758μg(r=0.9999);茶碱:0.0973~0.8759μg(r=0.9999);咖啡因:0.0614~0.5522μg(r=0.9999),平均回收率为可可碱:99.8%(RSD=0.6%,n=9);盐酸麻黄碱:100.4%(RSD=0.9%,n=9);茶碱:99.6%(RSD=0.5%,n=9);咖啡因100.1%(RSD=0.3%,n=9)。本方法简便、快速,专属性强,可有效地控制复方茶碱麻黄碱片中可可碱、茶碱、咖啡因和麻黄碱的含量。     

HPLC法测定复方羊角片中阿魏酸的含量

目的测定复方羊角片中阿魏酸的含量.方法采用高效液相色谱法.色谱柱为Kromasil C18色谱柱(4.6×250mm,5μm),以甲醇-0.1%醋酸溶液(30∶70)为流动相;流速:1.0mL·min-1,检测波长321nm.结果阿魏酸的进样量在0.08~0.28μg范围内呈良好的线性关系(r=0.9999),平均加样回收率为100.3%,RSD为1.71%(n=6).结论方法简便、准确,可用于复方羊角片中阿魏酸的含量测定.     

高效液相色谱法测定二维钙赖氨酸片中盐酸赖氨酸含量

目的探讨测定二维钙赖氨酸片中盐酸赖氨酸含量的方法。方法采用Luna C_(18)柱(250 mm×4．6 mm,5μm)为色谱柱,流动相为乙腈- pH值为7．0的磷酸盐缓冲液(30：70),检测波长为360 nm,流速为0．6 mL/min。结果盐酸赖氨酸进样量在0．15～3．00μg范围内与峰面积线性关系良好,r=0．9996,平均回收率为99．83%,RSD为0．37%。结论该方法灵敏快速,测定结果准确、重现性好,可用于该制剂的质量控制。     

HPLC法同时测定复方茶碱麻黄碱片中4组分的含量

目的:用高效液相色谱法同时测定复方茶碱麻黄碱片中可可碱、盐酸麻黄碱、茶碱和咖啡因的含量。方法:采用Diamonsil C18色谱柱(250mm×4.6 mm,5μm);流动相:甲醇-0.05 mol·L-1磷酸二氢钾溶液-三乙胺(25:75:0.1);流速:0.8 ml·min-1;检测波长:210nm。结果:可可碱进样量在0.06～0.39μg(r=0.999 6)、盐酸麻黄碱进样量在0.03～0.16μg(r= 0.999 6)、茶碱进样量在0.06～0.38μg(r=0.999 6)、咖啡因进样量在0.04～0.23μg(r=0.999 6)范围内呈良好的线性关系。平均回收率分别为100.3%(RSD=0.3%);100.2%(RSD=0.6%);100.2%(RSD=0.6%);100.7%(RSD=0.5%)。结论:本方法简便、准确、重现性好,可用于同时测定复方茶碱麻黄碱片中4组分的含量。     

HPLC测定海珠喘息定片中盐酸氯丙那林和盐酸去氯羟嗪的含量

目的建立高效液相色谱法同时测定海珠喘息定片中盐酸氯丙那林和盐酸去氯羟嗪的含量。方法色谱柱:AGTVenusil XBP-C18(250 mm×4.6 mm,5μm);流动相:甲醇-0.015 mol.L-1磷酸二氢钠(含0.15%三乙胺pH=3.1)(30∶70),梯度洗脱;检测波长:215 nm。结果盐酸氯丙那林和盐酸去氯羟嗪检的平均回收率在98.0%~100.3%,RSD<2%;线性范围分别为0.4~1.6μg,r=1.000 0(n=5)和2.1~8.3μg,r=0.999 9(n=5)。结论本法分离效果好,准确快速,适用于海珠喘息定片中盐酸氯丙那林和盐酸去氯羟嗪的含量测定。     

HPLC法测定复方茶碱麻黄碱片中四种组分的含量

目的:建立高效液相色谱法同时测定复方茶碱麻黄碱片中四种组分含量的方法。方法:采用Dismonsil(Dikma)C18(20cm*4.6mm,5μl)色谱柱,0.05mol/L磷酸二氢钾-甲醇-三乙胺(77:23:0.02)为流动相,流速为1.0ml/min,检测波长为215nm,柱温:40℃。结果:所选流动相适用范围较广,耐用性好,样品中四种组分均能达到良好的分离度。可可碱、盐酸麻黄碱、茶碱、咖啡因的浓度分别在5.392μg/ml～53.92μg/ml(r=1.0000)、4.894μg/ml～21.24μg/ml(r=1.0000)、2.124μg/ml～48.94μg/ml(r=1.0000)、2.98μg/ml～29.8μg/ml(r=1.0000)范围内线性关系良好。可可碱的平均回收率为100.1%(RSD=0.5%),盐酸麻黄碱的平均回收率为100.5%(RSD=1.0%),茶碱的平均回收率为100.2%(RSD=0.6%),咖啡因的平均回收率为100.1%(RSD=0.7%)。结论:本测定方法简便、准确、精密度高,可有效控制复方茶碱麻黄碱片中四种组分的含量。     

HPLC法同时测定氨麻苯美片中4种主要成分的含量

目的:建立同时测定氨麻苯美片中盐酸伪麻黄碱、对乙酰氨基酚、氢溴酸右美沙芬和盐酸苯海拉明等成分含量的HPLC方法。方法:色谱柱为Kromasil 60-5CN(25 mm×4.6 mm,5μm)柱;以乙腈-pH3.0的40 mmol.L-1三乙胺水溶液(20∶80)为流动相;检测波长为215 nm;流速为1.0 mL.min-1。结果:盐酸伪麻黄碱、对乙酰氨基酚、氢溴酸右美沙芬和盐酸苯海拉明的线性范围分别为6.036~150.9μg.mL-1(r=1.0000),65.42~1636μg.mL-1(r=0.9989),3.010~75.25μg.mL-1(r=1.0000),50.90~127.2μg.mL-1(r=1.0000);加样回收率(n=9)分别为98.5%,100.9%,99.1%和99.6%。结论:本法简单、快速、准确,可用于氨麻苯美片中4种主要成分的同时测定。     

HPLC法测定复方氨酚苯海拉明片中对乙酰氨基酚、咖啡因、盐酸麻黄碱和盐酸苯海拉明的含量

目的建立同一色谱条件测定复方氨酚苯海拉明片中的对乙酰氨基酚、咖啡因、盐酸麻黄碱和盐酸苯海拉明含量的HPLC法。方法采用苯基柱(4.6 mm×250 mm,5μm),流动相为甲醇-pH 3.5的10 mmol.L-1乙酸铵溶液(体积比85∶15),检测波长为225 nm。结果对乙酰氨基酚、咖啡因、盐酸麻黄碱和盐酸苯海拉明的分离度好,对乙酰氨基酚、咖啡因、盐酸麻黄碱和盐酸苯海拉明的回收率分别为100.1%、100.0%、100.2%和100.6%(n=9)。结论本方法操作简单,结果准确,可以有效地控制复方氨酚苯海拉明片的质量。     

毛细管气相色谱法测定复方丹参片中冰片含量

目的:建立复方丹参片中冰片的提取及气相色谱法测定含量的方法,了解该药品中冰片含量情况。方法:提取法:索氏提取和旋转蒸发法;测定法:色谱条件为 HP-CARBOWAX 20M 毛细管色谱柱(25m×0.32mm,0.52μm),柱温115℃,载气为氮气,分流比为60:1,FID 检测器,内标物为环己酮。结果:冰片的浓度在0.0375～2.305 mg·mL~(-1)范围内呈线性关系(r=0.9998),方法的回收率为95%,RSD 为2.2%(n=3)。结论:本方法可用于复方丹参片中冰片含量测定。     

HPLC—ELSD法测定盐酸赖氨酸葡萄糖注射液的含量

目的:建立高效液相色谱-蒸发光散射检测法测定盐酸赖氨酸葡萄糖注射液中盐酸赖氨酸及葡萄糖含量。方法:采用 Covasil-C_(18)柱(250 mm×4.6 mm,5μm),以0.05 mol·L~(-1)醋酸铵-甲醇-乙腈(1:1:1)为流动相,流速为0.5 mL·min~(-1)。蒸发光散射检测器(ELSD),漂移管温度为40℃,空气流速为1.5 L·min~(-1)。结果:在选定色谱条件下,盐酸赖氨酸、葡萄糖分别在0.3～0.65 g·L~(-1)(r=0.9997),1.5～3.15 g·L~(-1)(r=0.9994)范围内呈良好的线性关系,回收率分别为98.6%～100.3%,97.8%～99.5%。结论:本法简便,专属性好,可用于盐酸赖氨酸葡萄糖注射液中盐酸赖氨酸及葡萄糖含量检测。     

Degradation kinetic study of lysine in lysine hydrochloride solutions for injection by determining its main degradation product

A limited number of researches have been reported to apply the Arrhenius equation to study the relationship between drugs and its degradation products so far. In the present work, the thermal degradation kinetics of lysine hydrochloride solutions for injection, the special solvent for ademetionine 1, 4-butanedisulfonate (SAM) for injection, was investigated at selected temperatures and pH values. The main degradation product of lysine was separated, purified, and confirmed as lysine lactam. A reversed-phase high performance liquid chromatographic (RP-HPLC) method without derivation was developed for the simultaneous determination of lysine and lysine lactam. The results confirmed that both the lysine degradation and lysine lactam generation followed zero-order reaction kinetics. The degradation and generation rate constants increased with increasing temperatures and decreasing pH values. The temperature-dependent degradation and generation reaction could be sufficiently modeled on the Arrhenius equation with the activation energy of 80.14 and 83.22 kJ/mol, respectively. Meanwhile, a linear relationship existed between the amount of lysine degradation and lysine lactam generation since the approximate activation energy. Considering there could be other side effects, we established an upper limit of lysine lactam (500 μg/ml), as the acceptable criteria for stability to estimate the shelf life together with lysine, which made the prediction more accurate and credible. Extrapolation data demonstrated that the lysine hydrochloride solutions for injection could be stable for two years stored at room temperature.     

RP-HPLC法测定赖氨肌醇维B12口服溶液中盐酸赖氨酸的含量

目的 建立反相高效液相色谱检测方法赖对氨肌醇维B12口服溶液中盐酸赖氨酸的含量的方法.方法 优选盐酸横氨酸组份的柱前衍生条件及色谱条件.结果 在选定的柱前衍生条件和色谱条件下,盐酸赖氨酸的分析不受辅料和其他物质的干扰.结论 本方法专属性强,灵敏度高,可用于赖氨肌醇维B12口服溶液中盐酸赖氨酸的含量测定.     

Crystal and molecular structure of L-lysyl-L-valine hydrochloride – a new lysine conformation

Thin plates of L-lysyl-L-valine hydrochloride (C₁₁H₂₄N₃O₃Cl) were obtained using the vapour diffusion technique and analysed by X-ray diffraction. The unit cell is orthorhombic, space group P2₁2₁2₁, a = 5.465(6)Å, b = 19.657(4) Å, c = 13.522(2) Å, V = 1452.6(2.1) ų and Z = 4. The structure was solved by direct methods and refined to an agreement factor of 6.7% for 939 reflections with I > 3 σ(I). The lysine side chain conformation (g^- g^- tt) has never been found in peptide crystal structures, although it has been reported to occur in proteins. A network of hydrogen bonds between peptide molecules spreads along the a and c directions while no direct bonds are observed to occur between peptides along the b axis direction. This asymmetric pattern of interactions correlates with the crystal morphology.     

贯叶连翘提取物和盐酸赖氨酸抗疱疹病毒复方筛选

目的 :评价贯叶连翘提取物和盐酸赖氨酸复方抗疱疹病毒活性 ,有效复方在整体动物的安全性。方法 :(1 )采用细胞病变效应法 (CPE) ,测定贯叶连翘提取物与盐酸赖氨酸 3种复方 (分别以质量比 1∶1、1∶ 2和 2∶ 1配比 )对Vero细胞和 2BS细胞的细胞毒性 ,以及对单纯疱疹病毒I型 (HSV 1 )和水痘 带状疱疹病毒 (VZV)的抗病毒活性。 (2 )一次灌胃(ig)给予小鼠复方 (2∶ 1 ) ,观察 1 4d ,测定LD5 0 。结果 :贯叶连翘提取物和盐酸赖氨酸 3种复方体外对HSV 1和VZV表现不同程度的抗病毒活性 ,最小有效浓度(MIC)和半数有效浓度 (IC5 0 )范围分别为 9.7～1 9.5mg·L- 1和 6 .8～ 9.7mg·L- 1,测得复方 (2∶1 )单次小鼠ig的LD5 0 为 1 1 .7g·kg- 1,95 %置信区间为 6 .5～ 1 7.2g·kg- 1。结论 :贯叶连翘提取物和盐酸赖氨酸复方体外具有较好抗HSV I和VZV作用 ,2∶ 1复方属于无毒药物范围     

应用亲水作用色谱技术同时测定赖氨葡锌口服液中两有效成分的含量

目的：应用亲水作用色谱（HILIC）技术,建立可同时测定赖氨葡锌口服液中葡萄糖酸锌和盐酸赖氨酸含量的方法。方法：色谱柱为Inertsil Amide柱（250 mm×4.6 mm,5 μm）,以磷酸盐缓冲液（取磷酸二氢钾2.72 g,辛烷磺酸钠0.46 g,加水1 000 mL使溶解）-乙腈（32∶68）为流动相A,以磷酸盐缓冲液（取磷酸二氢钾2.72 g,辛烷磺酸钠0.46 g,加水1 000 mL溶解）-乙腈（95∶5）为流动相B,（梯度洗脱,0~2 min,100% A;2~15 min,100% A→100% B;15~17 min,100% B）,检测波长203 nm,柱温30℃。结果：在选定的色谱条件下,葡萄糖酸锌峰和赖氨酸峰分离度良好,葡萄糖酸锌和盐酸赖氨酸分别在0.364 8~3.648 1和0.406 5~4.605 0 mg·mL^-1浓度范围内具有良好的线性关系,平均回收率（n=3）在97.97%~101.97%之间。结论：建立的方法可有效控制赖氨葡锌口服液的质量,也可为质量标准改进提供新的研究思路。     

赖氨葡锌治疗小儿急性腹泻的效果分析

目的 探讨赖氨葡锌治疗小儿急性腹泻的效果.方法 选择2009年1月～2012年12月来本院治疗的小儿急性腹泻患者100例,随机分为实验组（50例）与对照组（50例）,实验组行对症支持治疗加赖氨葡锌治疗,对照组仅给予对症支持治疗,比较两组的疗效.结果 实验组有效率高于对照组,住院时间明显短于对照组,两组差异有统计学意义（P＜0.05）.结论 赖氨葡锌能显著提高小儿急性腹泻的治疗效果,且安全可靠.     

Levalbuterol hydrochloride

Racemic salbutamol (racemic albuterol) ameliorates symptoms of asthma by activating b-adrenoceptors on nerve, smooth muscle and inflammatory cells within the airways. Racemic salbutamol comprises equal proportions of 2 isomers: (S)-salbutamol and (R)-salbutamol, with the latter being exclusively responsible for activation of b-adrenoceptors. Accordingly, within racemic salbutamol it is (R)-salbutamol that efficiently relieves obstruction of asthmatic airways and affords highly effective protection from bronchoconstrictor stimuli, including allergens. During regular use of racemic salbutamol, there is a progressive decline of protective efficacy and a corresponding intensification of airway responsiveness. This decline is largely absent during regular use of (R)-salbutamol. Consequently, bronchodilator responses to sub-maximal doses of (R)-salbutamol exceed responses to the equivalent dose of (R)-salbutamol given as the racemate. For example, in asthmatics with baseline FEVs ≤ 60%, 1.25 mg of nebulised (R)-salbutamol achieved a maximal 52% change in FEV while 2.5 mg of racemic salbutamol only achieved a 38% change in FEV. Since extrapulmonary effects (e.g., tremor, heart rate) of b agonists are related to dose and limit the use of b agonist therapy, (R)-salbutamol at 0.63 mg provides uncompromised efficacy with marked reduction of side-effects. In addition to quantitative differences, the constituent isomers of salbutamol also exhibit qualitative differences. Thus, (R)-salbutamol inhibits activation of human eosinophils in vitro whereas, under the same conditions and concentrations, (S)-salbutamol augments activation of these cells. This property of (S)-salbutamol may explain why eosinophilia in induced sputum from subjects with allergic asthma is increased by regular use of racemic salbutamol. Similarly, the capacity of (R)-salbutamol to suppress hyperresponsiveness of the airways can be contrasted with the capacity of (S)-salbutamol to intensify hyperresponsiveness. This action of (S)-salbutamol would explain why regular use of racemic salbutamol intensifies the bronchoconstrictor response to antigen in subjects with allergic asthma. Taken together, these findings imply that replacement of racemic salbutamol by (R)-salbutamol will diminish, or even eliminate, the anomalous actions that have curtailed the efficacy of racemic salbutamol. Pharmacokinetically, (R)-salbutamol exhibits near absolute conformational stability (i.e., no conversion to (S)-salbutamol). If in vitro anti-inflammatory actions of (R)-salbutamol are also manifest in asthmatic airways, (R)-salbutamol could provide a novel approach to asthma therapy which combines bronchodilation and bronchoprotection with anti-inflammatory efficacy.