高效液相色谱法测定扑米酮中的杂质苯巴比妥含量

采用高效液相色谱法测定扑米酮中特殊杂质苯巴比妥的含量。色谱柱μ-Bondsphere C_(18)(3.9mm×150mm,5μm)流动相为甲醇-水(18:32),检测波长254nm。线性范围为0.05～0.3μg(n=5,r=0.9998),平均回收率为100.2％(n=5,RSD=1.737％)。     

HPLC法对八珍益母丸中芍药苷和阿魏酸的含量

目的 ：建立八珍益母丸中芍药苷和阿魏酸含量测定的方法。方法 ： 采用高效液相色谱法,色谱柱为Kromasil C₁₈柱 (250mm?4.6mm,5μm);乙腈—0.1%磷酸(18：82)为流动相;流速为1.0m L.min_-1;柱温35℃;检测波长为 230。结果：芍药苷在0.06492～0.6492 μg (r=0.9992 n=6 ),平均回收率为99.52%(RSD 1.53%,n=6);阿魏酸在0.02652.～0.2652μg范围内线性关系良好(r=0.9996 n=6),平均回收率为103.70%(RSD 0.99%,n=6)。 结论：该方法操作简单,分离度高,回收率好,适用于八珍益母丸的质量控制。     

高效液相色谱法测定香砂养胃丸中厚朴酚与和厚朴酚的含量

目的:建立和改进香砂养胃丸含量测定方法。方法:以Hypersil ODS C_(18)(5μm,150 mm×4.6mm)色谱柱分离厚朴酚 与和厚朴酚,流动相乙腈-水-冰醋酸(50:8:2),检测波长294nm。结果:线性范围:厚朴酚1.12～5.60μg,r=0.9999(n=5),和厚朴酚0.8288～4.144μg,r=0.9999(n=5)。厚朴酚平均回收率99.1％,RSD=1.64％(n=5),和厚朴酚平均回收率102.4％,RSD=1.67％(n=5)。结论:本法简便,快速,准确,可作为该制剂质量控制的方法。     

HPLC法测定头孢呋辛酯及其片剂的含量

建立头孢呋辛酯及其片剂的含量测定方法。以岛津Shim-Pack C₁₈(4.6 mm×150 mm,5μ)色谱柱,以0.2 mol/L磷酸二氢铵溶液-甲醇(62:38)为流动相,以278 nm为检测波长。线性范围为0.05～2 mg/ml,回归方程为Y=2.69×10⁶X-1.87×10⁵,r=0.9999,平均回收率为99.4％(RSD=0.9％,n=9)。     

非那西丁及其代谢产物对乙酰氨基酚的高效液相色谱测定

目的　建立非那西丁及其代谢产物对乙酰氨基酚的高效液相色谱测定方法。方法　色谱柱:Nova Pak^RC₁₈(3.9mm×15 0mm ,5 μm) ;流动相为甲醇水溶液,其梯度洗脱程序为:17% (体积分数,下同)甲醇(保持5min)→80 %甲醇(10min)→17%甲醇(12min) ;检测波长2 5 4nm。结果　非那西丁、对乙酰氨基酚线性范围分别为0.687～87.920μg/mL(r=0.9999,n=5) ,0.423～54.200μg/mL(r==0 .9997,n=5)。低、中、高三种浓度的平均方法回收率非那西丁为96.9% (n=5) ,对乙酰氨基酚为95 .1% (n=5 ) ;日内,日间精密度(RSD)均小于6 % (n=5 )。结论　本研究为非那西丁的药物代谢研究提供了一种测定方法。     

紫外分光光度法测定复方异烟肼片中维生素

After isoniazid was extracted with acetone, vitamine B₆ was determined in hydrochloric acid(0.1mol/L) at wavelength of 291nm.Beer's law is obeyed in the concentration range of 6～18μg/ml.The average recovery is 99.6% (RSD=0.41%, n=5), Suggesting our result is satisfactory.     

高效液相色谱法测定四消片中大黄素及大黄酚的含量

目的:建立高效液相色谱法测定四消片中大黄素及大黄酚的含量。方法:选用 KRO-MASIL C_(18)分析柱(150×4.6mm)5μm,流动相为甲醇—0.1％磷酸溶液(85∶15),检测波长254nm。结果:大黄素在4.184～41.84μg/mL(γ=0.9999,n=5),大黄酚在21.08～210.8μg/mL(γ=0.9999 n=5)浓度范围内呈线性关系,大黄素和大黄酚平均回收率分别在99.36％和99.63％(RSD 分别为0.78％和1.01％)。结果:本法可用于四消片的定量检验。     

HPLC内标法测定注射用喷昔洛韦含量

目的:用HPLC内标法测定喷昔洛韦的含量。方法:以Spherisorb C_(18)柱为色谱分析柱,流动相为0.01mol·L~(-1)磷酸二氢钾一甲醇(90:10) ;内标物系对乙酰氨基酚;检测波长252nm。结果:喷昔洛韦的线性范围为25～75μg·ml~(-1),r=0.9999(n=5),回收率为98.6％,RSD=1.0％(n=6)。结论:本法含量测定结果满意。     

HPLC法测定野菊花中绿原酸的含量

目的;建立野菊花中绿原酸的含量测定方法并测定其含量。方法:用 50％甲醇回流提取;HPLC法测定,分析色谱柱为Inertsil C_(18)(5μm,4.6mm×150mm),流动相为乙腈-0.4％磷酸水溶液(12:88),UV346nm检测。结果:精密度试验批内(n=9)RSD为1.3％,批间(n=9)RSD为1.8％;平均回收率(n=5)为100.3％,RSD为2.0％。分析了3种市售样品,野菊花中绿原酸含量为0.33％～0.36％。结论:方法简便,可靠;绿原酸可作为野菊花的质量控制指标。     

加替沙星血药浓度HPLC测定方法研究

目的:建立加替沙星血药浓度的高效液相色谱分析方法。方法:以乳酸司帕沙星为内标,采用10％高氯酸为沉淀剂处理人血浆样品,分析柱为Phenomenex(Luna,C_(18),5μm粒径,150 mm×4.6 mm);Easyguard C_(18)保护柱。流动相为0.01mol·L~(-1)磷酸二氢钾缓冲液-乙腈 (18:5,用磷酸调pH为3.05),流速1.0 mL·min~(-1),柱温25℃,在292 nm波长处检测,按内标法定量。结果:血药浓度线性范围为0.025～8μg·mL~(-1)(r=0.999 9),最低检测浓度为0.025μg·mL~(-1)(S/N>3),萃取回收率在76.31％～87.70％(n=5),方法回收率在98.3％～102.3％(n=5),日内和日间RSD分别为3.3％～5.6％和4.8％～9.8％(n=5)。结论:本方法简便、准确,精密度高,重现性好,适用于加替沙星人体内药代动力学研究及生物等效性研究。     

治疗帕金森病新药:腺苷A_(2A)受体拮抗剂

腺苷A2A受体在基底神经节选择性表达并与运动行为有关。流行病学研究和实验室研究均表明阻断腺苷A2A受体能减轻多巴胺能神经元的退行性病变。腺苷A2A受体拮抗剂在改善PD症状的同时还能减缓疾病的进程。因此,腺苷A2A受体拮抗剂很可能成为治疗PD的新药物。     

葛根黄豆甙元-PVP分散物的研究

本文采用聚乙烯吡咯烷酮(PVP)为载体,制备了葛根黄豆甙元固体分散物。经差热分析、X-射线衍射、偏光显微镜观察实验证明黄豆甙元-PVP 1∶9固体分散物为固体溶液或共沉淀物,其胶囊在人工胃液中最高累积释放百分量和人工肠液中平衡溶解度均是普通胶囊的8倍左右。     

SCH 58261: A selective A2A adenosine receptor antagonists

The recent discovery of selective antagonists for the A_2A adenosine receptors has been of great help to further research in this field. One compound, SCH 58261, 5- amino-7-(β-phenylethyl)-2-(8-furyl)pyrazolo[4,3-e]-1,2,4-triazolo[1,5-c]pyrimidine, is playing a key part in a variety of studies. This review describes its pharmacological characteristics as they are emerging in various laboratories. The compound has an affinity in the low nM range (Ki value of 1–2 nM) for A_2A receptors located on membranes from a variety of tissues and cell types, including rat and bovine brain striatum, human platelets, lymphocytes and neutrophils, porcine coronary arteries, and CHO cells transfected with the cloned human A_2A receptors. SCH 58261 has little or no affinity up to the μM range for adenosine A_2B, A₃, or other G protein-coupled receptors. Selectivity for A_2A vs. A₁ receptors varies from 53- to 750-fold, depending on membranes or type of assay. SCH 58261 blocks A_2A-receptor mediated increase of cyclic AMP formation with high potency (e.g., IC₅₀ values between 15 and 20 nM in human white blood cells). The tritiated form of SCH 58261 specifically labels A_2A receptors in discrete regions of the rat brain such as caudate-putamen, nucleus accumbens, and tuberculum olfactorium. In classic in vitro bioassays, such as A_2A-receptor-mediated vasodilation in coronary arteries, SCH 58261 displays competitive antagonistic properties (e.g., pA₂ value of 9.5 in porcine coronary arteries). In assays involving responses mediated by A₁ or A_2B receptors, SCH 58261 shows little or no activity up to concentrations about 100-fold higher than those affecting A_2A receptors (higher concentrations not being testable due to its poor water solubility). In the rat, SCH 58261 enhances locomotor activity (at 3.7 mg/kg ip), increases wakefulness (10 mg/kg ip) and slightly increases both blood pressure and heart rate (10 mg/kg ip). These activities appear to be specifically mediated by A_2A receptors since the drug counteracts the effect of A_2A receptor agonists in some experimental paradigms. In models mimicking CNS disorders, SCH 58261 potentiates the activity of L-DOPA or dopamine receptor agonists in the 6-hydroxydopamine-lesioned rat model. Moreover, the compound reduces brain infarct size in a rat model of cerebral ischemia. Altogether, SCH 58261 and its radiolabeled form have emerged as interesting tools for better understanding the function of A_2A receptors in physiological or altered conditions. Moreover, the neuroprotective properties of SCH 58261 indicate that drugs of this class have a potential for treatment of brain damage produced by Parkinson's disease or stroke. Drug Dev. Res. 42:63–70, 1997. © 1997 Wiley-Liss, Inc.     

β-淀粉样蛋白和载脂蛋白E4升高神经元胞内游离钙

目的　研究 β 淀粉样蛋白 (Aβ)和载脂蛋白E4(ApoE4)对神经元胞内游离Ca2 +浓度的影响 ,探索它们对神经元的毒性效应。方法　制备 0～ 3d新生SD大鼠的海马和皮层神经元悬液 ,负载上fura 2 /AM ,实验组分别加入Aβ2 5～ 3 5、ApoE4以及Aβ2 5～ 35+ApoE4孵育液温孵 3min后 ,用荧光双波长分光光度计测定神经元 [Ca2 +]i;采用显微准弹性激光散射技术 (MQLS) ,分析Aβ2 5～ 35及ApoE4对单个神经元散射光强度自相关函数 (ACF)的影响 ,通过公式由ACF拟合出反映细胞膜流动性的频移线宽Г。结果　Aβ2 5～ 35和ApoE4均能升高海马和皮层神经元静息 [Ca2 +]i(P <0 0 5 ) ,其中 5 μmol·L-1Aβ2 5～ 35的作用大于 1μmol·L-1Aβ2 5～ 3 5的作用 (P <0 0 5 ) ;Aβ2 5～ 35和ApoE4也能增强KCl去极化诱导的海马和皮层神经元 [Ca2 +]i 升高 (P <0 0 5 )。Aβ2 5～ 3 5(1μmol·L-1) +ApoE4(0 1μmol·L-1)共同作用也使神经元静息 [Ca2 +]i及KCl去极化诱导的神经元 [Ca2 +]i升高 (P <0 0 5 ) ,但两者共同作用未见其升 [Ca2 +]i 效应进一步增大。Aβ2 5～ 3 5和ApoE4均降低海马和皮层神经元的频移线宽Г。结论　Aβ2 5～ 35和ApoE4均能升高神经元静息[Ca2 +]i 及降低神经元膜流动性 ,但两者共同作用未能显示升 [C