HPLC-UV测定不同产地及不同采收期酸枣叶中芦丁的含量

目的:考察不同产地及不同采收期酸枣叶中芦丁的含量,以确定其最佳采收期,为酸枣叶的资源开发提供科学依据。方法:采用HPLC,Diamonsil(钻石)C18色谱柱(4.6 mm×200 mm,5μm),流动相甲醇-0.1%冰醋酸(34∶66),检测波长257nm,流速1.0 mL.min-1,柱温30℃。结果:芦丁在0.221 6～2.216μg有良好的线性关系(r=0.999 9),平均加样回收率为99.40%(RSD 2.42%,n=6);酸枣叶中芦丁含量一般以5～6月含量最高,7～8月芦丁含量有所下降,9～10月又有所升高。结论:酸枣叶中芦丁的含量整体上随时间变化基本呈U字形趋势,该方法准确、简便、稳定,为酸枣叶的质量标准提供参考。     

HPLC-UV法测定苯丁酸钠片的含量及有关物质

目的 建立HPLC-UV法测定苯丁酸钠片的含量及有关物质.方法 采用高效液相色谱仪,C18色谱柱(250 mm×4.6 mm,5 μm),流动相:乙腈-5 mmol·L-1磷酸溶液(40:60),柱温40℃,检测波长:215 nm,流速:1.0 ml· min-1,进样:20 μl.结果 苯丁酸钠在21.14～105....     

生千金子鉴别研究(英文)

目的:研究建立具有抗癌等特殊药理活性的毒性药材生千金子(Semen Euphorbiae)的鉴别分析方法。方法:采用形态鉴别、显微鉴别、液相色谱及液质联用技术进行研究。HPLC-UV条件:C18(250 mm×2.1 mm,5μm);流动相为乙腈-磷酸盐缓冲液,梯度洗脱:流速为200μL.min-1;进样量20μL;检测波长275 nm。LC-MS/MS条件:PE-SCIEX API-300LC-MS-MS系统;流动相为乙腈-甲酸缓冲液,梯度洗脱;进样10μL。其他同前。结果:本文利用所建立的方法对4个不同产地的药材进行了分析。液相色谱及液质联用分析方法主要测定药材中秦皮乙素、千金子甾醇、续随子醇二乙酸二苯甲酸酯、续随子醇二乙酸苯甲酸酯、续随子醇二乙酸吡啶甲酸酯等有效成分。结论:本文研究结果可为进一步验证药材质量提供参考。     

Bioequivalence evaluation of a triamterene-hydrochlorothiazide generic product: a new bioequivalence index for fixed-dose combinations

In this study, an open, double-blind, randomized, two-period, two-group crossover design was conducted in 14 healthy volunteers to study the bioequivalence of a fixed-dose generic product. After administration of test or reference products to each volunteer, both active ingredients were determined simultaneously in plasma samples using a developed and validated HPLC-UV method, and pharmacokinetic parameters, including C(max), T(max), AUC(0-t) , AUC(0∞), terminal elimination rate constant (λz), volume of distribution in steady state (Vd(ss)), mean residence time (MRT), clearance (Cl), terminal elimination rate constant (Kel) were determined in each subject using the standard non-compartmental approach. Statistical comparison showed that the test and reference products were bioequivalent in terms of both the rate and extent of bioavailability of both active ingredients. Finally, a new parameter named range overlap index (ROI) was introduced for the first time in this study in order to judge about the overall bioequivalence of the combination products. This parameter indicates the extent in which the two CI90% ranges of each parameter for two active ingredients overlap with each other. The ROI is suggested to be equal or more than 50% for two combination products in order to be known as bioequivalent. The ROI values of the bioequivalence-indicating parameters were 61.90%, 84.6%, and 76.0% for C(max), AUC(0--->12), and AUC(0--->∞), respectively, which are indicative for bioequivalence in all the cases.     

HPLC—UV法用于人血浆中罗红霉素的浓度测定及药代动力学和生物等效性研究

目的建立HPLC-UV法测定人血浆中罗红霉素的方法,并探讨罗红霉素的药代动力学和生物等效性。方法采用Diamonsil C18柱（150mm×4．6mm,5μm）,流动相为乙腈：0．01mool磷酸二氢铵=39：61（v／v）,流速1mL／min;以卡马西平为内标,检测波长为210nm。血浆样品用正己烷（含5％的异丙醇）液-液萃取后经C18分离。结果罗红霉素在0．25～16．0mg／L线性关系良好,r=0．999,最低检测限为0．25mg／L。萃取回收率〉70％,方法回收率99．8％～110．5％,批内、批间精密度均〈15％。结论HPLC—UV方法结果准确、灵敏度高,适用于罗红霉素药代动力学和生物等效性研究。     

基于UPLC-DAD-TOF/MS结合HPLC-UV法的麻黄“先煎去沫”样品的化学成分分析

目的建立基于UPLC-DAD-TOF/MS结合HPLC-UV法检测麻黄样品化学成分的方法,以明确麻黄"先煎去沫"样品化学成分间的差异。方法 UPLC-DAD-TOF/MS:Waters ACQUITY UPLC?BEH C18(50 mm×2.1 mm,1.7μm)色谱柱,以甲醇-0.1%甲酸水溶液为流动相梯度洗脱,体积流量0.3 m L/min,柱温40℃,正、负离子模式扫描;HPLC-UV:以十八烷基硅烷键合硅胶为填充剂(150 mm×4.6 mm,5μm),以0.1%磷酸水溶液(含0.05%三乙胺)-乙腈溶液(99∶1)为流动相,等度洗脱,体积流量1 m L/min,检测波长为210 nm,柱温30℃。结果上沫中所含成分较少,去沫下液和全煎煮液中化学成分基本一致。同时,三者均可鉴定出去甲基麻黄碱、去甲基伪麻黄碱、麻黄碱、伪麻黄碱和甲基麻黄碱5个生物碱类成分和1个羧酸类成分(4-羟基-7-甲氧基-2-喹啉羧酸)。但上沫中生物碱含量极低,而全煎煮液中3种生物碱的含量略高于去沫下液。结论麻黄"先煎去"沫理论可能与生物碱类成分关系不大,但仍需后期进行更深入的研究验证。     

Analysis of Imazaquin in Soybeans by Solid-phase Extraction and High-performance Liquid Chromatography

An analytical method for the determination imazaquin residues in soybeans was developed. The developed liquid/liquid partition and strong anion exchange solid-phase extraction procedures provide the effective cleanup, removing the greatest number of sample matrix interferences. By optimizing mobile-phase pH water/acetonitrile conditions with phosphoric acid, using a C-18 reverse-phase chromatographic column and employing ultraviolet detection, excellent peak resolution was achieved. The combined cleanup and chromatographic method steps reported herein were sensitive and reliable for determining the imazaquin residues in soybean samples. This method is characterized by recovery >88.4%, precision <6.7% CV, and sensitivity of 0.005 ppm, in agreement with directives for method validation in residue analysis. Imazaquin residues in soybeans were further confirmed by high performance liquid chromatography-mass spectrometry (LC-MS). The proposed method was successfully applied to the analysis of imazaquin residues in soybean samples grown in an experimental field after treatments of imazaquin formulation.     

HPLC—UV检测北细辛及数种中成药中的马兜铃酸A

目的：检查北细辛药材及数种中成药中的马兜铃酸A。方法：采用高效液相色谱法,紫外检测器,以Hypersil C18柱（250mm×4．6mm,5μm）测定马兜铃酸A的含量,流动相为甲醇-水-二甲基甲酰胺-冰醋酸（25：13：1：1,v／v）,流速1．0mL·min^-1,检测波长315nm,柱温35℃。结果：在所选定的色谱条件下,细辛药材及含细辛药材的中成药未检出马兜铃酸A。结论：该检测方法测得马兜铃酸A最低检出量为1．8×10^-4μg,为马兜铃酸A的检测提供了一种灵敏、经济、可行的科学方法。北细辛药材及含细辛药材的中成药中均未检出马兜铃酸A。     

HPLC-UV法测定大鼠脑组织中5-羟色胺含量

目的建立大鼠脑组织中5-羟色胺(5-HT)含量的HPLC-UV测定方法。方法采用SHIMADZU VP-ODS C18反相柱(250×4.6mm,5μm),流动相:甲醇-0.01mol/L的醋酸钾缓冲液(10:90,V/V,用0.2mol/L柠檬酸调pH至4.00);流速:1.0ml/min;柱温:25℃;检测波长:275nm。结果 5-羟色胺在0.1～20μg/ml范围内,回归方程为A=46008.89C+1886.58,相关系数r=0.9999,最低检测限为40ng/ml,最低定量限为100ng/ml。加样回收率为89.62%～101.60%,日内、日间精密度均小于3%。结论该方法准确可靠,简单易行,可重复性强,适用于多样本5-HT的快速测定。     

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。