高效液相色谱法测定马拉韦罗片的含量

目的建立高效液相色谱法测定马拉韦罗片的含量。方法色谱柱:Shimadzu C18柱(250 mm×4.6 mm,5μm),流动相:乙腈-0.01 mol.L-1磷酸二氢钾溶液(25∶75,V/V),柱温:(35.0±1.0)℃,流速:1.0 mL.min-1,检测波长:197 nm。结果马拉韦罗的线性范围为0.1～0.5 g.L-1(r=0.999 7),平均回收率为(99.83±0.60)%(n=9)。结论本方法简便、准确,可用于马拉韦罗片的含量测定。     

反相高效液相色谱法测定盐酸乙哌立松片剂的含量

目的：建立高效液相色谱法测定盐酸乙哌立公片含量的方法。方法：酸盐乙哌立松片加甲醇,超声振荡,过滤后以ODS C18为分析柱,以甲醇－水－三乙胺（80：19．5：0．5,V／V）为流动相,托哌酮为内标,于254nm波长检测。结果：盐酸乙哌立松在0．4－1．6mg/ml浓度范围内线性关系良好（r=0.9999),平均回收率98．4％,RSD,1．2％,三批协酸乙哌立松片含量测定结果分别为标示量的97．8％,98．3％和98．9％,结论：方法快速,准确,专一性强,适用于盐酸乙哌立松片的含量测定。     

氯沙坦钾片的HPLC测定

目的:建立高效液相色谱法测定氯沙坦钾片含量,为质量控制提供有效的分析手段.方法:色谱柱:Phenomenex ODS C18(5μm、4.6mm×150mm);流动相:乙腈-0.1%磷酸溶液(55:45);检测波长:230nm.结果:制剂中辅料和有关物质对主药无干扰,氯沙坦钾在浓度100.2～350.8μg/mL范围内线性关系良好,相关系数r＝0.9999;平均回收率分别为99.36%、99.68%、99.40%,RSD为0.42%.结论:本法专属性好,准确,简便.     

HPLC法测定甲磺酸酚妥拉明分散片的含量

目的：建立了采用高效液相色谱法测定了一种药物新剂型甲磺酸酚妥拉明分散片的含量的方法。方法：采用Ｋromasil C18色谱柱,流动相为醋酸溶液（取冰醋酸１.0ml加水至１０00ml,用三乙胺调节pH值至3．8）－甲醇（10：90）, 检测波长设定在278nm。结果：线性范围为进样量0．2－5．0μg,r=0.9998,平均回收率为99．5％,RSD＝0．70％。结：本方法快速、无干扰、精密度好,灵敏度高。     

反相高效液相色谱法测定克拉霉素缓释片的含量

目的：用反相高效液相色谱法测定克拉霉素缓释片的含量。方法：采用ODS反相柱，流动相为乙腈：0．067mol/L，KH2PO4＝35:^65(H3PO4调节pH至3．5），结果：克拉霉素在辅料中的回收率为98．57％，进样，重复性实验，中间精密度的RSD分别为0．40％，0．77％，0．69％，结论：本法准确，快捷，适用于测定克拉霉素缓释片的含量。     

那格列奈片的高效液相色谱分析

目的:建立那格列奈片中主药那格列奈及杂质的高效液相色谱测定方法。方法:采用Shim-Pack CLC-ODS(150mm×6.0mm)色谱柱,甲醇-0.02mol.L~(-1)磷酸盐缓冲液(pH6.6)(75:25)作流动相,检测波长210nm,含量测定采用外标法, 杂质检查采用面积归一化法。考察了不同流动相下那格列奈的色谱行为及其与杂质的分离情况。结果:在优化的色谱条件下,片剂辅料不干扰测定,有关杂质与主药那格列奈分离良好,那格列奈线性范围5.1～101.0 mg·L~(-1),最低检测限0.2 mg·L~(-1),含量测定的回收率99.4％～100.4％,RSD<1.7％。结论:此法简便,准确,专属性强,重现性好,可用于那格列奈片的质量控制、稳定性考察和有效期预测。     

高效液相色谱法测定小儿泻痢停片中醋酸泼尼松的含量

目的建立小儿泻痢停片中醋酸泼尼松的高效液相检测法.方法色谱柱Hypersil ODS2(5μm,4.6mm×200mm),流动相甲醇-水(58∶42),流速1.0mL/min,检测波长240nm,氢化可的松为内标物.结果醋酸泼尼松和内标的保留时间分别为11.4min和7.5min.在80～240 μg/mL浓度范围内,醋酸泼尼松与内标峰面积之比与浓度呈良好的线性关系(r=0.9998),醋酸泼尼松平均回收率为99.95%,RSD为0.26%.结论用高效液相色谱法测定醋酸泼尼松的含量,简便、准确、灵敏度高,可用于该制剂的质量控制.     

高效液相色谱法测定托拉塞米片中托拉塞米及其有关物质的含量

目的:建立高效液相色谱法测定托拉塞米片中托拉塞米及其有关物质的含量。方法:以岛津ShimpackCLC(M)C18(250mm×4.6mm,5μm)为色谱柱;以甲醇-0.02mol·L-1磷酸二氢钾溶液(用磷酸调节pH至3.0)(65∶35)为流动相;UV检测波长291nm;流速0.9mL·min-1。结果:托拉塞米在2～24mg·L-1范围内具有良好线性关系(r=0.9999),平均加样回收率为99.73%,RSD为0.17%(n=9);3批样品的标示百分含量(%)分别为99.80,100.10,100.40,有关物质的百分含量分别为0.58,0.45,0.39。结论:本方法准确、灵敏,重现性好,可用于托拉塞米片及其有关物质的含量测定。     

高效液相色谱法测定恩他卡朋片的含量

目的建立恩他卡朋片含量测定的方法。方法色谱柱:Intersil C18(4.6 mm×250 mm,5μm),流动相:甲醇-乙腈-0.03 mmol.L-1磷酸二氢钾缓冲溶液(磷酸调节pH至2.75)(35∶25∶40,V/V/V),检测波长:310 nm,柱温:30℃,流速:1.0 mL.min-1。结果恩他卡朋的线性范围为10～50 mg.L-1(r=0.999 9),平均回收率为(99.74±0.69)%,RSD=0.68%(n=9)。结论本方法简便、准确、重现性好,可用于恩他卡朋片的含量测定。     

Determination of pravastatin by high performance liquid chromatography

BACKGROUND: Pravastatin is a hydrophilic liver-specific inhibitor of the enzyme 3-hydroxy-3-methylglutaryl coenzyme A reductase. It effectively lowers plasma cholesterol and low-density lipoprotein concentrations in humans. Pharmacokinetic studies of pravastatin have been mostly performed by means of radioactively labelled drug or by measuring plasma concentrations with gas chromatography and mass spectrometry. AIMS OF THE STUDY: Aim of our study was to develop a simple, but reliable method which allows the determination of pravastatin plasma concentrations under clinical routine conditions. SUBJECTS, MATERIALS AND METHODS: Samples were prepared by solid-phase extraction on cyclohexyl bond elut cartridges. Chromatography was carried out on an octyl matrix. Triamcinolone acetonide was used as internal standard. The method was linear within the range of 5 to 200 microg/l pravastatin. The coefficient of variation depended on the pravastatin concentration, but was less than 10% throughout. The pharmacokinetics of pravastatin were determined in healthy individuals. Five healthy subjects received single oral doses of pravastatin (60 mg) and one of these subjects additionally received a dose of 80 mg at three different study days. In all subjects blood was sampled 0, 30, 60, 90, 120, 150, 180, 240 and 300 min after drug intake. RESULTS: Peak plasma concentrations of pravastatin were found between 60 min and 120 min after oral administration of 60 mg and reached values between 37 microg/l and 126 microg/l. The calculated AUCs were between 52 ng/ml x h and 311 ng/ml x h and the corresponding plasma elimination half-life times were between 95 min and 165 min. In all subjects plasma concentrations of pravastatin 5 hours after oral drug administration were near the detection limit of the method (5 microg/l). Intraindividually, there was only little variation in the kinetics of pravastatin. However, marked differences were encountered between the subjects studied. CONCLUSION: The data suggest that the determination of pravastatin plasma concentrations by means of a HPLC system can be used for routine analysis of pravastatin plasma concentrations. The obtained pharmacokinetic data in healthy individuals stand in ample agreement with the results of prior studies in which the concentrations of pravastatin were determined by other more sophisticated methods.     

正相高效液相色谱法测定多维片类保健食品中维生素 A的含量

目的：建立多维片类保健食品中维生素A含量测定方法。方法色谱柱：Phenomenex Luna silica（2）（250 mm ×4．6 mm,5μm）,流动相：正己烷—异丙醇（99．7∶0．3）,流速：1．0 mL· min－1,检测波长：325 nm,柱温：室温。结果维生素A在9．27～185．33 ng范围内峰面积与进样量呈良好线性关系,r＝0．9999,平均回收率为97．8％,RSD为2．4％（ n＝9）。结论该方法操作简便、准确,可用于控制多维片类保健食品中维生素A的质量。     

高效液相色谱法测定三磷酸腺苷二钠含量

目的建立三磷酸腺苷二钠含量的测定方法。方法采用高效液相色谱法 ,以弱碱性离子交换球状硅胶为固定相 ;检测波长 2 5 9nm ;流动相为磷酸盐缓冲液 (pH 7.0 ) ;柱温 35℃。结果此法可将三磷酸腺苷二钠与一磷酸腺苷、二磷酸腺苷二钠盐分离。结论该法专属性强 ,灵敏、快速     

高效液相色谱法测定莫西沙星制剂含量

目的 :建立高效液相色谱法测定莫西沙星制剂的含量。方法 :采用InertsilODS 2色谱柱 (5 μm ,2 5 0mm× 4.0mm) ,流动相为 1%三乙胺溶液 (磷酸调pH值至 4.5 )—乙腈 (84∶16,v/v) ;柱温 :40℃ ;检测波长 :2 96nm ;流速 :1.0ml/min。结果 :线性范围 0 .4～ 3 μg ,r =0 .9999,平均回收率为 10 0 .7% (RSD =0 .7% )。结论 :方法简单 ,专属性好 ,可用于莫西沙星制剂的含量测定。     

HPLC法测定淫羊藿苷微乳的含量

目的 建立高效液相色谱法测定淫羊藿苷微乳的含量.方法 采用色谱柱:ASMKromasil C18(150 mm×4.6 mm,5μm);流动相:乙腈-水(体积比30∶70:):流速:1.0 ml·min-1;检测波长:270 nm;柱温:25℃.结果 淫羊藿苷在0.55～1.45μg范围内的线性关系良好,r=0.9996.加样回收率为99.12％,RSD为0.32％.结论 本测定方法快捷、简便、准确,可用于淫羊藿苷微乳的质量控制.     

高效液相色谱法测定血浆中法莫替丁的浓度

目的:用高效液相色谱法测定血浆中法莫替丁浓度。方法:以对乙酰氨基酚为内标,血浆经乙腈提取,HPLC测定。流动相0.01m o l.L-1磷酸二氢钾-乙腈(91.5:8.5),流速1.0m l.m in-1,C 18色谱柱A lltech A po llo(4.6mm×150mm),检测波长266nm。结果:法莫替丁和内标与内源性杂质分离良好;5~160 ng.m-l 1浓度范围内线性关系良好;检测限2.5 ng.m-l 1;日内精密度RSD为1.5%~6.7%(n=6),日间精密度RSD为0.2%~14%(n=6)。结论:本法简便、灵敏度较好,可用于法莫替丁血药浓度的测定。     

用高效液相色谱法测定兔血清中硫酸庆大霉素的含量

本文以高效液相色谱法测定血清中硫酸庆大霉素的含量。加内标物茴香胺。乙腈沉淀蛋白质等干扰物，室温下进行邻苯二醛衍生化，醋酸乙酯提取后进样，用紫外３３０ｎｍ检测。     

Determination of clonazepam in serum by high performance liquid chromatography

A simple, specific, and sensitive high-performance liquid chromatography (HPLC) method has been developed for the routine monitoring in serum of the benzodiazepine anticonvulsant, clonazepam. Serum spiked with internal standard, methylclonazepam, was vortex-mixed for 1 min with chloroform at an alkaline pH. The evaporated extract was dissolved in the HPLC mobile phase consisting of sodium phosphate buffer, acetonitrile, and methanol. Analytics were resolved at ambient temperature on a 5-micron Supelcosil LC-PCN column (150 X 4.6 mm) equipped with a guard column. Flow rate was 2.0 ml/min, and monitoring was at 306 nm. The calibration curve was linear from 2 to 200 ng/ml. This method provides selectivity and sensitivity with a precision of 3.5%, average recovery of 99%, and no interference from 42 commonly administered drugs.     

高效液相色谱法测定米非司酮的血药浓度

目的　建立测定米非司酮血药浓度的方法。方法　以乙腈∶水 (70∶3 0 )为流动相 ,炔诺酮作内标 ,血浆样品经用乙醚萃取后上样 ,经C18柱分离后 ,在紫外波长 3 0 2nm处检测米非司酮 ,在 2 40nm处检测炔诺酮。结果　线性范围 0 .0 5～ 10 .0 μg·mL-1(r =0 .9995 )。平均相对回收率在 95 %～ 110 %之间 ,日内和日间RSD均小于 6%。米非司酮最低检出限为 0 .0 1μg·mL-1,萃取回收率大于 90 %。结论　本法快速、简便、准确、灵敏 ,可用于米非司酮的药物动力学研究     

高效液相色谱法测定交沙霉素血药浓度

目的建立测定人体内血清中交沙霉素(Jos)浓度的方法.方法采用改进的HPLC法,色谱柱为SUPELCODiscovery