高效液相色谱法测定人血浆中西洛他唑的浓度

目的 :建立以高效液相色谱法测定人血浆中西洛他唑浓度的定量分析方法。方法 :色谱柱为迪马公司C18(150mm×4 6mm ,5μm ) ,流动相为乙腈 -水 (40∶60 ,V/V ) ,流速为1 4ml/min ,检测波长为254nm。结果 :西洛他唑检测浓度在25～2000ng/ml范围内线性关系良好 (r=0 9999),最低检测浓度为12 5ng/ml ,回收率为99 .99 %～101 .44 % ,日内、日间相对标准差分别为0 .20 %～2 90 %、0. 19 %～2. 13 % (n=5)。结论 :本方法简便、快捷、灵敏、准确 ,可用于西洛他唑人体药动学研究。     

HPLC法测定人血浆中西洛他唑的浓度

目的建立测定人血浆中西洛他唑浓度的HPLC法。方法以迪马公司钻石C18反相柱(250 mm×4.6 mm,5μm)为色谱柱,流动相为甲醇-0.03 mol.L-1醋酸铵(62∶38,V/V),流速0.8 mL.min-1,检测波长257 nm,以乙酸乙酯为提取剂。结果西洛他唑高(1 000μg.L-1)、中(500μg.L-1)、低(25μg.L-1)3种质量浓度的平均回收率分别为99.51%、97.07%、98.28%,日内、日间RSD均<7%;分析方法的最低检测浓度为10μg.L-1。线性范围为10~1 500μg.L-1。结论该方法灵敏、准确、简单、快速,可用于西洛他唑临床血药浓度监测和药动学研究。     

高效液相色谱法测定人血浆中西洛他唑浓度

目的:建立测定人血浆中西洛他唑浓度的高效液相色谱法.方法:西洛他唑血浆样品以2 mol·L -1 氢氧化钠-无水乙醚(1∶4)提取,以地西泮为内标.Hypersil C 18 柱( 4.6 mm×200 mm, 5 μm),流动相为乙腈-水 (45∶55),流速: 1.0 mL·min -1 ,检测波长:285 nm.结果:标准曲线线性范围 20.0 ～ 1 200.0 μg·L -1 (r= 0.999 9 ).血浆中西洛他唑最低检测限为10 μg·L -1 .平均提取回收率为( 81.52 ± 3.81 )%,平均方法回收率( 97.4 ± 4.5 )%, 日内及日间RSD均<11%.结论:所建立的HPLC方法灵敏、专一、准确、精密,简便,适用于西洛他唑的药动学研究及治疗药物浓度监测.     

HPLC-MS/MS法测定人血浆中西洛他唑浓度

目的建立灵敏快速检测人血浆中西洛他唑浓度的HPLC-MS/MS方法。方法采用色谱柱为Thermo Hy-purity C18（150 mm×2.1 mm,5μm,USA）,流动相为乙腈（含0.1%甲酸）-甲醇=25∶75（v/v）;流速为0.2mL.min-1;ESI＋离子源,MRM进行离子方式监测。质谱参数：源电压3 500V,源温度100℃,去溶剂化温度350℃,锥孔气流速50 L.h^-1,去溶剂化气流速350 L.h^-1;血浆处理采用乙腈直接沉淀萃取方法。结果血浆中西洛他唑检测方法的线性范围为4.90-2 510 ng.mL-1,最低检出浓度为4.90 ng.mL-1,血浆中西洛他唑的方法回收率在80%-120%,日内RSD〈10%,日间RSD〈15%。结论本方法用于测定人血浆中西洛他唑的浓度,简单、快速、灵敏。     

反相高效液相色谱法测定西洛他唑胶囊的含量

目的建立反相高效液相色谱法测定西洛他唑胶囊剂的含量。方法选用XTerra RP18（4.6mm×250mm,5μm）为色谱柱,甲醇—水（0.68∶0.32）为流动相,流速为1.0ml/min,检测波长为257nm,柱温为30℃。结果西洛他唑的浓度在19.92～99.60μg/ml范围内线性关系良好（r=0.9999,n=5）,平均回收率为100.60%（n=6）,相对标准偏差为0.65%（n=6）。结论本方法简便、灵敏、准确,可用于西洛他唑胶囊的质量控制。     

高效液相色谱法测定人血浆中西洛他唑药物浓度及药动学研究

目的建立高效液相色谱法测定人血浆中西洛他唑的浓度,并研究其在健康人体内的药动学。方法采用C18反相色谱柱,以乙腈-水(0.1%甲酸)(65∶35)为流动相等度洗脱,流速为1.0 mL·min-1;检测波长为257 nm;进样量为20μL。结果西洛他唑在0.05～10 mg·L-1范围内线性关系良好(r=0.999 8),各样品的提取回收率均大于80%,日内、日间精密度RSD均小于10%。西洛他唑的血药经时过程符合一级吸收的二室模型,其主要药动学参数:tmax:2.94±1.21 h;Cmax:(0.99±0.12)mg·L-1;AUC(0-t):(9.57±1.31)mg·h-1.L-1。结论该方法方便快捷,专属性强,准确可靠,适用于西洛他唑的临床药动学研究。     

HPLC法测定人血浆中伏立康唑的浓度

目的:建立一种快速、灵敏、准确、稳定的测定人血浆中伏立康唑浓度的方法,用于伏立康唑临床治疗药物监测。方法:采用高效液相色谱(HPLC)-紫外检测法,以卡马西平为内标,乙腈蛋白沉淀法处理血浆样品。色谱柱为Phecda C18,流动相为20mmol/L磷酸二氢钾缓冲液(p H=6.0)-乙腈(50∶50,V/V),流速为1 ml/min,柱温为40℃,检测波长为255 nm,进样量为50μl。结果:伏立康唑和卡马西平的保留时间分别为8.34和6.24 min;血浆中伏立康唑线性范围为0.10~20.00μg/ml(r=0.999 5),定量下限为0.05μg/ml,日内、日间RSD分别为≤1.57%、1.45%,低、中、高梯度浓度提取回收率在81.40%~128.29%之间。结论:该方法操作简便,结果准确,适用于伏立康唑的临床治疗药物监测。     

反相高效液相色谱法测定人血浆中利鲁唑浓度

目的 :建立测定利鲁唑血药浓度的方法。方法 :采用反相高效液相色谱法 ,以DiamonsilTM C18(250mm×4. 6mm ,5μm )为色谱柱 ,甲醇 -0 .03mol/L磷酸二氢铵 (80∶20 ,V/V)为流动相 ,乙醚为提取剂 ,流速为0. 8ml/min ,检测波长为265nm。结果 :利鲁唑检测浓度线性范围为5～1000ng/ml ,最低检测浓度为5ng/ml ;高、中、低3种浓度的回收率分别为99 .51 %、95. 74 %和97. 12 % ,日内RSD≤1 .17 %、日间RSD≤6. 48 % (n=5)。结论 :本方法灵敏、准确、简单、快速 ,可用于人体药动学研究。     

HPLC法测定西洛他唑分散片含量

目的:建立高效液相色谱法测定西洛他唑分散片的含量.方法:采用DOS柱,以腈-水(40:60)为流动相257 nm波长处检测.结果:西洛他唑浓度在8～72μg·ml-1范围内有良好的线性关系(r=0.999 9,平均回收率为99.8%.结论:本法快速,准确.     

西洛他唑的高效液相色谱法测定及药动学研究

目的 :建立测定人血浆中西洛他唑含量的高效液相色谱 (HPLC)法 ,并研究西洛他唑片在健康人体内的药动学。方法 :色谱柱为HypersilC18柱(4 .6mm× 2 0 0mm ,5 μm) ,流动相为乙腈 水 (4 5∶5 5 ) ,流速 1.0ml·min-1,柱温 30℃ ,检测波长2 5 4nm ,西洛他唑血浆样品以 2mol·L-1NaOH 无水乙醚 (1∶4 )提取 ,以地西泮为内标。结果 :标准曲线线性范围 2 0～ 2 0 0 0 μg·L-1(r =0 .9999)。血浆中西洛他唑最低检测限为 10 μg·L-1。平均提取回收率为 80 .2 %± 3.6 % ,平均方法回收率为 97.0 %±3.8% ,日内RSD≤ 5 .8% ,日间RSD≤ 10 .1%。应用该法研究了 10例健康志愿者口服 10 0mg西洛他唑后的药动学 ;其体内过程符合二室模型 ,tmax为 3.5 8± 1.0 8h ,Cmax为 92 0± 2 30 μg·L-1,AUC0 -48为 11.0± 3.3mg·h-1·L-1。结论 :此法简便、快速 ,适用于药物分析 ,其药动学数据可为临床合理用药、新药研制及剂型改进提供理论依据     

反相高效液相色谱法测定人血清中西洛他唑质量浓度

目的建立测定人血清中西洛他唑质量浓度的反相高效液相色谱（RP—HPLC）法。方法采用液-液萃取高效液相色谱紫外检测法,以地西泮为内标,色谱柱为Phenomenex Synergi 4u Fusion—RP C18柱（250mm×4．6mm,5μm）,流动相为乙腈-水（45：55）,流速1．0mL／min,检测波长258nm。结果血清中内源性物质不干扰西洛他唑的检测,西洛他唑质量浓度的线性范围为0．016～2．000μg／mL,日内、日间精密度的RSD均小于15％,低、中、高质量浓度（0．031,0．250,1．000μg／mL）溶液的平均提取回收率分别为76．8％,78．5％,77．1％。结论RP—HPLC法快速、简单、准确,符合生物样品检测要求,可用于临床药代动力学研究。     

Determination of cilostazol and its metabolites in human urine by high performance liquid chromatography

A high performance liquid chromatography (HPLC) method with ultraviolet detection for the simultaneous quantification of cilostazol, and its known metabolites in human urine was developed and validated. Cilostazol, its metabolites and the internal standard OPC-3930 (structural analogue of cilostazol) were extracted from human urine using liquid-liquid extraction with chloroform. The organic extract was then evaporated and the residue was reconstituted in 8% acetonitrile in ammonium acetate buffer (pH 6.5). The reconstituted solution was injected onto an HPLC system and was subjected to reverse-phase HPLC on a 5-microm ODS column. A gradient mobile phase with different percentages of acetonitrile in acetate buffer (pH 6.5) was used for the resolution of analytes. Cilostazol, its metabolites and the internal standard were well resolved at baseline with adequate resolution from constituents of human urine. The lower limit of quantification was 100 ng/ml for cilostazol and all metabolites. The method was validated for a linear range of 100-3000 ng/ml for all the metabolites and cilostazol. The overall accuracy (% relative recovery) of this method ranged from 86.1 to 116.8% for all the analytes with overall precision (%CV) being 0.8-19.7%. The long-term stability of clinical urine samples was established for at least 3 months at -20 degrees C in a storage freezer. During validation, calibration curves had correlation coefficients greater than or equal to 0.995 for cilostazol and the seven tested metabolites. The method was successfully used for the analysis of cilostazol and its metabolites in urine samples from clinical studies, demonstrating the reliability and robustness of the method.     

Hydrolytic Degradation Profile and RP-HPLC Estimation of Cilostazol in Tablet Dosage Form

A simple, selective, precise and stability-indicating high-performance liquid-chromatographic method of analysis of cilostazol in pharmaceutical dosage form was developed and validated. The solvent system consisted of 10 mM phosphate buffer (pH 6.0):acetonitrile:methanol (20:40:40). Retention time of cilostazol in C18 column was 5.7 ± 0.1 min at the flow rate 1.3 ml/min. Cilostazol was detected at 248 nm at room temperature. The linear regression analysis data for the calibration plots showed good linear relationship with correlation coefficient value, r ² =0.9998 in the concentration range 100–3200 ng/ml with slope 43.45 intercept 156.75. The method was validated for linearity, range, accuracy, precision and specificity. Cilostazol was determined in tablet dosage form in range of 99.58-100.67% with 0.4600 standard deviation. Stress studies were conducted in acid and alkali hydrolysis with gradual increasing concentration. Cilostazol was found to be stable in various concentrations of acidic and alkaline.     

反相高效液相色谱法测定大蒜素的血药浓度

目的：建立反相高效液相色谱法测定血清中大蒜素的浓度。方法：血清样品用１０％三氯醋酸沉淀蛋白,正己烷提取后进样。采用Ｐｈｅｎｏｍｅｎｅｘ Ｃ１８（２５０ｍｍ × ４．６ｍｍ,５μｍ）柱;流动相：乙腈－１％冰醋酸（６２：３８,Ｖ／Ｖ）,ｐＨ＝３．５;流速：１．２ｍｌ／ｍｉｎ,在室温下;波长：２４０ｎｍ检测。结果：该方法回收率为（９９．２±６．６）％,最低检测浓度为０．１８μｇ／ｍｌ,大蒜素血药浓度在０．２９～１２．４μｇ／ｍｌ范围内峰面积与浓度线性关系良好（ｒ＝０．９ ９７７）,日内 ＲＳＤ＜５．５％（ｎ＝５）,日间 ＲＳＤ＜５．８％（ｎ＝５） 结论：本法快速、准确、灵敏,能较好满足大蒜素临床药代动力学研究的需要。     

A validated method for the determination of verapamil and norverapamil in human plasma

The aim of the study was to develop a simple and sensitive analytical method to determine verapamil (V) and its metabolite norverapamil (N) in human plasma with use of an HPLC isocratic system with fluorescence detection, following fast extraction of the investigated compounds. Extraction recovery was 92.12% and 89.58% for V and N, respectively. Internal standard in HPLC was propranolol. Its recovery was 82.50% on the average. Limit of detection was 0.924 ng/ml and limit of determination was 3,080 ng/ml for V, what corresponds concentration in plasma 1.232 ng/ml. For N limit of detection was 0.030 ng/ml and limit of determination was 1.001 ng/ml what corresponds 0,4 ng/ml in plasma. Parameters of validation prove that precision of the presented method is very good. The method is fast and one chromatogram separation lasts about 8 minutes. 30-40 manual (without autosampler) analyses per day were done. It was used successfully in pharmacokinetic and bioavailability studies of verapamil administration in drug formulations alternative to tablets: buccal and flotation ones.     

高效液相色谱-质谱法测定人血浆中非洛地平浓度

目的:建立以高效液相色谱-质谱法测定人血浆中非洛地平浓度的方法。方法:采用高效液相分离系统,流动相为甲醇-水-醋酸,流速为1ml/min,分流比2∶1,固定相为HypersilC18柱;采用质谱检测系统,AP-ESI正离子模式,雾化压力0.054Pa(400psi),保护气N210L/min,毛细管电压4000V,离子源温度100℃,碎片电压为220V,离子采集方式为SIM,采集离子为非洛地平m/z411(M+Na),尼莫地平m/z441(M+Na)。结果:非洛地平检测浓度线性范围为0.2～50ng/ml,最低检测限为0.15ng/ml,回收率在90.93%以上,日内、日间RSD均<9.8%。结论:本法灵敏度高,适用于非洛地平治疗药物监测及其药动学和生物利用度研究。     

反相高效液相色谱法测定血清中头孢他美浓度

目的 :以反相高效液相色谱法测定血清中头孢他美浓度。方法 :血清样品经甲醇沉淀蛋白 ,10000r/min离心15min后取上清液直接进样。色谱分析条件 :hypersilBDSC18(4 6mm×150mm ,5μm) ;流动相 :甲醇∶水=28∶72(V/V ,pH2 8) ;流速 :1 0ml/min ;柱温 :室温 ;检测波长 :262nm。结果 :血清中头孢他美在0 53～13 25μg/ml浓度范围内线性关系良好 ,最低检出浓度为0 25μg/ml,平均方法回收率为100 84 % ,日内RSD≤4 42 % ,日间RSD≤4 17 %。结论 :本法简便、灵敏、准确可靠 ,可用于头孢他美的体内药代动力学研究。