高效液相色谱-紫外分光光度法测定奥美沙坦酯片剂的含量及有关物质

目的采用高效液相色谱法测定奥美沙坦酯片的含量及有关物质。方法采用美国Alltech C18色谱柱(150 mm×4.6 mm,5μm),以0.1%甲酸水溶液-乙腈(67.5∶32.5)为流动相;流速为1.0 mL/min;柱温为25℃,波长为254 nm,进样量为10μL。结果含量测定的线性范围为0.50～10.00μg/mL,r=0.999 5(n=5),加样回收率为101.1%,99.5%,98.3%;RSD依次为1.2%,0.7,0.3%(n=5)。结论该方法简便快速、准确,专属性好。     

HPLC-UV技术用于川木香煨制前后代谢物轮廓差异研究

目的 比较川木香煨制前后代谢物轮廓(metabolic profiling)差异,筛选出导致差异的特征性化学成分.方法 经HPLC-UV分析获得川木香生品、煨品的色谱图数据集;采用主成分分析(principal component analysis,PCA)、偏最小二乘法-判别分析(partial least square-discriminant analysis,PLS-DA)、聚类分析(hierarchical cluster analysis,HCA)等多变量统计分析方法比较川木香生品、煨品的代谢物轮廓差异及筛选导致差异的特征性化学成分.结果 川木香生品和煨品代谢物轮廓明显不同,导致差异的特征性化学成分有7个(包含木香烃内酯和去氢木香内酯).结论 从代谢物轮廓角度,川木香煨制前后具有显著差异.     

Pharmacokinetics of Furegrelate After Oral Administration to Normal Humans

Furegrelate sodium is a thromboxane synthetase inhibitor with potential for the treatment of various diseases including hypertension, thrombosis, and renal disorders. The absorption and disposition of the parent drug in normal male volunteers have been studied after single- and multiple-dose oral administration. The results from the single-dose study indicate that furegrelate is rapidly absorbed, with a T _max of 1.0–1.7 hr, has an apparent terminal disposition rate constant of 0.12–0.17 hr^–1, and is eliminated primarily by the kidney, with 62–78% of the dose excreted as parent drug. After multiple-dose oral administration for 4.5 days using a b.i.d. dosing regimen, no apparent change in the absorption, disposition, and elimination kinetics is detected and only a slight potential for drug accumulation is observed.     

黄连解毒汤各成分的HPLC-UV/MS定性与定量测定方法研究

目的建立可整体定性、多指标定量的黄连解毒汤的分析方法。方法使用HPLC-UV/MS方法,梯度洗脱黄连解毒汤样品及组方各药单煎样品,归属色谱峰来源,并对主要色谱峰进行定性、定量分析。采用Zorbax Extend C₁₈(150 mm×4.6 mm ID,5 μm)色谱柱;流动相Ａ为乙腈,Ｂ为水(含0.5%冰醋酸),流速1 mL·min^-1。紫外检测波长254 nm,正、负离子扫描获得质谱数据。结果归属了21个色谱峰的来源,发现两个可区分黄连、黄柏的特征峰,通过HPLC-UV/MS对其中11个主要色谱峰进行了指认,并以HPLC-UV对8种有对照品的成分进行含量评价。结论黄连解毒汤与组方各药单煎样品有较好相关性,建立的方法所测得液相色谱图特征性和专属性强,该方法结合含量测定为黄连解毒汤内在质量控制提供了更全面的信息。     

基于HPLC-UV和FT-NIR的不同贮藏年限余甘子质量评价与鉴别

目的:探寻不同贮藏年限余甘子有效成分变化规律,为其保存策略提供理论依据。方法:采集7个不同贮藏年限的余甘子材料,高效液相色谱紫外光谱(HPLC-UV)测定没食子酸、柯里拉京、诃黎勒酸、鞣花酸、槲皮素的含量,阐明其主要活性成分累积特征;傅立叶变换近红外光谱(FT-NIR)记录样品整体光谱指纹图谱,偏最小二乘判别(PLS-DA)模型鉴别不同贮藏年限余甘子样品。结果:2015年版《中国药典》指标性成分没食子酸含量最高,其次是鞣花酸与诃黎勒酸,柯里拉京与槲皮素的含量较少;各成分在不同贮藏年限间样品中具有显著性差异(P0.05),没食子酸和槲皮素均在贮藏6年时达最大值,分别为79.36和1.68 mg·g~(-1),贮藏4年样品中诃黎勒酸、柯里拉京、鞣花酸累积最高,分别是18.85,7.97,21.46 mg·g~(-1)。MSC+SG二阶求导(窗口参数为11,多项式次数为3)优化FT-NIR数据,不同贮藏年限样品的分类正确率为84.5%;以最低交叉验证均方根误差为准则,降维光谱数据为若干重要潜在变量并与5种活性成分含量数据融合,鉴别正确率提高到98.8%。结论:基于HPLC-UV和FT-NIR技术,该研究有效阐述不同贮藏年限余甘子5种主要代谢成分累积特征;结合数据融合策略,PLS-DA模型能较好鉴别不同质量样品。该结果可为不同贮藏年限余甘子的质量鉴别及评价提供一定的科学依据。     

Development and Validation of a HPLC Method for the Determination of Cyclosporine A in New Bioadhesive Nanoparticles for Oral Administration

A simple and reliable high performance liquid chromatography method was developed and validated for the rapid determination of cyclosporine A in new pharmaceutical dosage forms based on the use of poly (methylvinylether-co-maleic anhydride) nanoparticles. The chromatographic separation was achieved using Ultrabase C₁₈ column (250×4.6 mm, 5 μm), which was kept at 75°. The gradient mobile phase consisted of acetonitrile and water with a flow rate of 1 ml/min. The effluent was monitored at 205 nm using diode array detector. The method exhibited linearity over the assayed concentration range (22-250 μg/ml) and demonstrated good intraday and interday precision and accuracy (relative standard deviations were less than 6.5% and the deviation from theoretical values is below 5.5%). The detection limit was 1.36 μg/ml. This method was also applied for quantitative analysis of cyclosporine A released from poly (methylvinylether-co-maleic anhydride) nanoparticles.     

Identification,isolation, characterization and response factor determination of process-related impurity in meprobamate drug substance

This paper describes identification and characterization of a process-related impurity of meprobamate drug substance observed in HPLC-UV method. Forced degradation studies were carried out under acidic, basic, oxidation, light and thermal conditions to assess the nature of the impurity. The pure impurity was obtained by preparative LC isolation and analyzed by NMR and mass. Structural elucidation by spectral data and formation of this impurity were discussed in detail. The structure of the process-related impurity was established as carbamic acid-2-carbamoyloxymethyl-2-methyl-pent-3-enyl ester (olefin). Also, the relative response factor, linearity, detection limit (DL), quantitation limit (QL) and recovery were determined for meprobamate and the impurity. Good linearity was obtained for the impurity over the concentration range of 0.03–0.20% (w/w) with the coefficient of determination (r²) of 0.999. The DL and QL of olefin impurity were 0.0003 and 0.001% (w/w), respectively. The isolated impurity was co-injected with meprobamate sample to confirm the retention time in HPLC.     

Quantitative Determination of α-Tocopherol in Globularia alypum Using High-Performance Liquid Chromatography with UV Detection

A quantitative determination of α-tocopherol in Globularia alypum L. was established by high-performance liquid chromatography (HPLC)-UV method. The investigations were carried out to evaluate the α -tocopherol content of the extracts from the air-dried aerial parts and the leaves of the plant. The calibration curve was used to calculate the content of the α-tocopherol, which was estimated as 0.002% and 0.0007% on the dried weight of the leaves and the aerial parts of G. alypum.     

高效液相色谱-紫外检测法测定利奈唑胺在体外药效学模型的浓度

目的 建立高效液相色谱-紫外检测法测定利奈唑胺(抗菌药)在国产肉汤基质的药物浓度.方法 MH肉汤样品350 μL,加入15%高氯酸沉淀蛋白,离心后取上清液50μL进样测定.Venusil XBP C_8(4.6 mm×250 mm,5 μm)色谱柱,流动相为水-乙腈(80∶20),流量为1.5 mL·min~(-1),紫外检测波长251nm,室温;用高效液相色谱-紫外检测法测定利奈唑胺浓度.结果 线性范围0.5～40.0 μg·mL~(-1)(γ=0.9996),低、中、高浓度的绝对回收率均大于90%,相对回收率在96%～98%,日内、日间RSD分别小于2%和4%;最低检测浓度为0.5 μg·mL~(-1).结论 该方法准确可靠、操作简便、灵敏度高,适用于体外药效学模型中药物浓度测定.