高效液相色谱法测定血浆中洛美沙星浓度及其在人体内药代动力学

建立了人血浆洛美沙星的反相离子对高效液相色谱测定方法。该法简便易行,精密度好,方法回收率95～102%,日内、日间RSD为2.1～7.8%,血药浓度在0.125～5.012 μg/ml范围内呈线性关系,相关系数0.9998,当S/N=2时,最小检测浓度为25 ng/ml。健康志愿者口服400 mg洛美沙星,药代动力学过程符合一室模型,消除相半衰期为5.5 h。     

高效液相色谱法测定奥美拉唑血药浓度及其药代动力学

建立了用反相高效液相色谱法测定血浆中奥美拉唑含量的分析方法。该分法采用液相提取预处理血样,在25～2000 ng/ml的浓度范围,线性关系良好,最低检测浓度4 ng/ml,奥美拉唑的相对回收率(98.07±5.21)％,日内变异<3.0％,日间变异<8.5％。并且,应用本法对正常人静脉推注奥美拉唑进行了药代动力学研究。     

高效液相色谱法测定人血浆中盐酸氨溴索的浓度及其药代动力学研究

目的 :建立测定盐酸氨溴索血药浓度的方法及进行人体药代动力学的研究。方法 :采用反相高效液相色谱法 ,色谱柱 :Phe nomenex C18 色谱柱 (5μm ,250mm×4 6mm) ,柱温 :室温 ,以乙腈 -甲醇 -0 01mol/L磷酸盐缓冲液 ( pH=7 0) -四氢呋喃 (35∶35∶27 5∶2 5v/v)为流动相 ,以西替利嗪为内标 ,流速1 5ml/min ,紫外检测波长242nm ,用盐酸氨溴索与内标的峰面积比进行定量。线性范围640～10μg/L ,最低检测浓度为5μg/L。对12名健康受试者单次口服90mg盐酸氨溴索片剂后的药代动力学进行研究。结果 :12名健康受试者的血药浓度数据经3p97拟合 ,符合血管外给药一室模型 ,AUC0～t 为 (2240 67±798 48) μg/(h·L) ,Cmax 为(253 17±65 11) μg/L ,Tpeak 为 (2 22±0 68)h ,T1/2ke 为 (4 18±1 27)h。结论 :方法简便 ,灵敏度和准确度较高 ,完全能满足人体内低浓度药物的测定及药代动力学研究的要求。     

高效液相色谱法测定美西律血清浓度和正常人药代动力学研究

本文报道了HPLC法测定抗心律失常药美西律血药浓度,方法灵敏、快速,并以此法研究8名正常成人单剂量口服美西律药代动力学。本测定方法以安定为内标物,流动相为甲醇和磷酸盐绥冲溶液(pH5.25),固定相为ODS(10μm),紫外检测器波长210nm。美西律和内标物的保留时间分别为5.49min和6.78rnin。在0.2～5μg/ml浓度范围与两者峰面积之比呈线性关系,y=0.7184x-0.064,r=0..9998。在三个浓度水平测得结果天内和天间变异系数均小于5％,回收率为94.3—99.6％。8名健康志愿者一次口服美西律片(100mg×3),其药——时曲线以一室开放模型拟台,并以此求算药代动力学参数,结果如下:K_a=1.328±0.634h~(-1);t_(112)=7.07±2.42h;V_d=6.23±2.22L/kg;Cl=0.509±0.157L/kg/h;T_(max)=2.79±0.71h;C_(max)=0.927±0.371μg/ml;AUC=11.723±4.870μg·h/ml。男、女间无显著性差异(p>0.1)。     

反相高效液相色谱法测定血浆中布洛芬浓度

目的 :建立反相高效液相色谱法测定血浆中布洛芬浓度的方法。方法 :以邻 羟基联苯作内标 ,10 %三氯醋酸沉淀蛋白 ,二氯甲烷 异丙醇混合溶剂 (5 0∶2 )提取 ,6 0 %甲醇和 40 % 0 1mol·L-1醋酸钠缓冲液 (pH 5 0 )作为流动相反相层析 ,检测波长 2 30nm。以布洛芬与内标峰面积比进行定量。结果 :布洛芬标准曲线A =0 30 98c 0 112 9,线性范围 1～ 30 μg·mL-1,r =0 9995 ,最低检测浓度为 0 1μg·mL-1。日内、日间RSD均 <6 % ,提取回收率均 >88%。结论 :本法简便、灵敏 ,为测定血浆中布洛芬浓度提供了方法     

反相高效液相色谱法测定环胞霉素全血浓度及药代动力学

环胞霉素(cyclosporine)是由11个氨基酸组成的一种环状多肽,具有选择性的免疫抑制作用,目前国内外已广泛用于各种器官移植及骨髓移植。环胞霉素口服吸收不完全,消除半衰期长,体内个体差异大,文献报道其相对生物利用度可从7.6～47.6%。环胞霉素血浓度过高将引起肝肾毒性及其他毒性反应,血浓度太低则影响疗效,病人将会出现排斥反     

高效液相色谱法测定人血浆中阿莫西林浓度及药代动力学

高效液相色谱法测定人血浆中阿莫西林浓度及药代动力学谭力周继红罗楠袁倚盛（南京军区南京总医院中心仪器分析科，南京２１０００１）阿莫西林（ａｍｏｘｉｃｉｌｉｎ）为β内酰胺类抗生素，其抗菌谱广，口服受食物影响小，对大多数病人耐受性良好，因而在临床上得以广泛...     

反相高效液相色谱法测定普萘洛尔血药浓度及药代动力学的研究

This paper investigates the determination method of propranolol in human plasma by HPLC. YWG-C₁₈H₃₇ column was used with CH₃OH-H₂O-0.2mol/L KH₂PO₄ 0.2mol/L Na₂HPO₄(460:40:0.7:4.7)as mobile phaseThe preparation of plasma sample: Transfer 0.5 ml plasma into a 5 ml polystyrene test tube with cap, add 0.8 ml of 0.2% sodium hydroxide solution into the plasma. Propranolol was extracted with ether. External standard was used for quantitation.The assay was evaluated using the reproducibility within day and day-to day, and demonstrated high precision. Their average coefficients of variation were 5.8% and 6.8% respectively. The standard curve was linear (r=0.9999)over the range of 0.05～2.00μg/ml, the average recovery was 95.9±4.5%.     

高效液相色谱法测定人血清中二甲胺四环素的浓度及其药代动力学研究

建立了反相高效液相色谱法测定二甲胺四环素的血药浓度。柱C18；以己腈-0．lmol／L枸橼酸溶液（15：85）为流动相，在353nm处测定。以土霉素为内标，血样在pH6．5条件下用乙酸乙酯提取；用二甲胺四环素与内标的峰高比进行定量。线性范围0．5～7μg／ml（Y=0．9994），最低检测限50ng／ml；平均回收率92．84％；日间RSD＜5％。应用本法研究了8名健康志愿者单次口服200mg盐酸二甲胺四环素胶囊后的药代动力学，符合二室开放模型，于2．4h达血峰浓度3．42±0．63μg／ml；AUC为77．12±16．89mg．h／L；t1/2为20．61±3．22h。     

反相高效液相色谱法测定普萘洛尔血药浓度及药代动力学的研究

普萘洛尔(propranolol)为β-受体阻滞剂,临床上被广泛用于治疗心律失常和心绞痛,有效浓度为50～150 ng/ml,也有报道为20～50 ng/ml。近来有报道口服普萘洛尔治疗血管性偏头痛。由于普萘洛尔的首过肝脏作用,生物利用度的个体差异大,有效剂量的变化也大。临床上希望通过测定普萘洛尔血药浓度,进行药代动力学过程的研究,结合临床指征,建立合理的用药方案。     

RP-HPLC法测定人体液中他唑巴坦浓度及其药动学应用

目的 :建立测定体液中他唑巴坦浓度的 HPLC方法 ,并应用于哌拉西林 /他唑巴坦健康人体的药代动力学研究。方法 :10名男性健康志愿者单剂量静脉滴注 4.5 g哌拉西林 /他唑巴坦钠 ,采用反相高效液相色谱 ( RP-HPLC)法测定血浆样品和尿中他唑巴坦药物浓度。 结果 :滴注完成即刻浓度 ( cm ax)为 ( 3 4.3 3± 8.0 5 )μg/m l,清除半衰期 ( t1 /2β)为 ( 0 .94± 0 .16) h,分布容积 ( Vd)为 ( 15 .43± 3 .82 ) L/kg,清除率 ( Clr)为 ( 15 .2 0± 2 .5 4) L /h,血药浓度 -时间曲线下面积 ( AUC)为 ( 4 2 .41±7.45 ) h·μg· ml-1 。结论 :他唑巴坦的体内过程符合二室开放模型 ,他唑巴坦主要以原形经肾脏排出体外 ,8h累积尿排百分率为 ( 78.68± 5 .84) %。     

Improved RP-HPLC method to determine biapenem in human plasma/urine and its application to a pharmacokinetic study

Existing methods to determine biapenem (CAS 120410-24-4), a carbapenem, either lacked sensitivity/reproducibility or had no internal standard as a control. Here an improved reversed-phase high-performance liquid chromatographic (RP-HPLC) method was established in human plasma and urine. After adding p-aminobenzoic acid as the internal standard to plasma or urine, plasma samples were ultra-filtrated and urine samples were diluted directly. Chromatographic separations were carried out on a 4.6 mm x 150 mm column with acetonitrile-0.1 mol/l sodium acetate (2:98, v:v; pH 4.38 or 4.00) as mobile phase and UV detection at 300 nm. The extraction recovery was 91.51% for biapenem at the concentration level of 5 microg /ml in human plasma. The linear quantification range of the method was 0.1 to approximately 50 microg /ml for plasma and urine, with linear correlation coefficients greater than 0.998. The intra-day and inter-day relative standard deviations (R.S.D.) for biapenem at low, middle and high levels in human samples were less than 12.51% for plasma and less than 7.05% for urine. The RP-HPLC method was successfully applied to pharmacokinetic studies, in which healthy subjects received multiple doses of biapenem (300 mg, i.v., b.i.d., for 5 continuous days). The pharmacokinetic results are presented.     

反相高效液相色谱法测定西替利嗪血药浓度及其在药动学研究中的应用

目的：建立测定西替利嗪在人体血浆中浓度的反相离子对高效液相色谱法（ＲＰ－ＨＰＬＣ）。方法：以Ｎｏｖａ－ＰａｋＣ１８４μｍ色谱柱为分离柱，流动相为乙腈∶磷酸盐缓冲液（０．０２ｍｏｌ·Ｌ－１ＮａＨ２ＰＯ４）∶三乙胺（５０∶５０∶０．１５，ｐＨ３．１５，内含十二烷基硫酸钠（ＳＤＳ）０．００９５ｍｏｌ·Ｌ－１，普萘洛尔为内标，ＵＶ检测波长２２９ｎｍ。结果：方法线性范围１０～４００ｎｇ·ｍｌ－１（ｒ＝０．９９９８），平均回收率为９８．１％±０．８％，日内和日间精密度均小于３％。结论：应用本法研究西替利嗪片剂在正常人体内的药动学，具有简便、迅速、准确之特点     

HPLC method for the determination of rosiglitazone in human plasma and its application in a clinical pharmacokinetic study

Rosiglitazone (CAS 155141-29-0, Avandia) is a novel insulin sensitizer used in the treatment of type 2 diabetes. A sensitive high performance liquid chromatography (HPLC) method for its determination in human plasma using fluorescence detection (excitation: 247 nm, emission: 367 nm) with a suitable internal standard (I. S.) is described. Ethyl acetate was used as extraction solvent. A mobile phase consisting of phosphate buffer, acetonitrile and methanol was used at a flow rate of 1.0 ml/min on a C18 column. The absolute recovery was > 90% and the lower limit of quantitation was 5 ng/ml. The intra- and inter-day relative standard deviations ranged from 0.58-6.69% and 0.82-6.63%, respectively. The method described is simple, economical, precise and accurate and has been successfully applied in a pharmacokinetic study conducted in healthy human volunteers.     

HPLC method for the determination of fluvoxamine in human plasma and urine for application to pharmacokinetic studies

A simple, specific and sensitive high-performance liquid chromatographic (HPLC) method has been developed for the assay of fluvoxamine in human plasma and urine. The method was based on reaction of fluvoxamine with 1,2-naphthoquinone-4-sulphonic acid sodium salt (NQS) forming orange colored product. The fluvoxamine-NQ derivative was separated by isocratic reversed-phase HPLC and detected at 450 nm. The chromatographic conditions were as follows: Phenomenex C(18) (250 mm x 4.6 mm i.d., 5 microm) column, mobile phase consisting of acetonitrile/water (80:20 v/v) at a flow rate of 1 ml/min. Tryptamine was selected as an internal standard. The assay was linear over the concentration range of 5-145 and 2-100 ng/ml for plasma and urine, respectively. The limits of detection (LOD) were 1.4 and 1 ng/ml for plasma and urine estimation at a signal-to-noise (S/N) ratio of 3. The limits of quantification (LOQ) were 5 and 2 ng/ml for plasma and urine, respectively. The extraction recoveries were found to be 96.66+/-0.69 and 96.73+/-2.17% for plasma and urine, respectively. The intra-day and inter-day standard deviations (S.D.) were less than 1. The method indicated good performance in terms of specificity, linearity, detection and quantification limits, precision and accuracy. This assay was demonstrated to be applicable for clinical pharmacokinetic studies.     

RP-HPLC法测定人血浆中拉莫三嗪及药动学

目的建立RP-HPLC法测定人血浆中的拉莫三嗪,并将此方法应用于拉莫三嗪片在健康受试者体内的药动学研究。方法血浆样品经乙酸乙酯提取后,采用Kromasil C18柱分离,流动相为乙腈-20 mmol.L-1 KH2PO4(体积比为25∶75),流速为1.0 mL.min-1,检测波长为306 nm。测定了11名健康受试者口服拉莫三嗪片50 mg后不同时刻血浆中拉莫三嗪的浓度,采用DAS 2.0软件以非房室模型计算药动学参数。结果拉莫三嗪的线性范围为10.0～2 000.0μg.L-1;日内和日间精密度均小于8.0%,准确度(relative error,RE)在±2.6%以内,提取回收率大于59.1%。拉莫三嗪的主要药动学参数:t1/2为(39.1±8.2)h,tmax为(3.3±1.8)h,ρmax为(469.6±152.4)μg.L-1,AUC0-t为(22 424.6±6 952.6)μg.h.L-1,AUC0-∞为(25 573.2±7 196.4)μg.h.L-1。结论该方法适用于拉莫三嗪人体药动学研究。     

RP-HPLC法测定人血浆中厄多司坦浓度及其药代动力学研究

目的:建立厄多司坦血浓度反相高效液相色谱测定方法,进行其人体药代动力学研究。方法:采用单剂两周期交叉试验设计,20名健康男性志愿者随机单剂量口服厄多司坦分散片或胶囊600 mg,按设定时间采集肘静脉血,以 Luna C_(18)(2)(150mm×4.6 mm,5 μm)为固定相,甲醇-醋酸钠(冰醋酸调 pH 至6.8)(5:95)为流动相,流速0.7 mL·min~(-1),检测波长236 nm,测定厄多司坦血浓度,计算其药代动力学参数,评价两制剂的生物等效性。结果:本方法最低定量限为0.01μg·mL~(-1),在0.01～3μg·mL~(-1)(r=0.9991)范围内线性关系良好,高、中、低浓度日内、日间 RSD 均小于5%。厄多司坦分散片和胶囊主要药代动力学参数 t_(1/2)分别为(2.478±1.206)h 和(2.603±1.282)h,T_(max)分别为(1.163±0.424)h 和(1.413±0.424)h,C_(max)分别为(1.419±0.385)μg·mL~(-1)和(1.594±0.558)μg·mL~(-1),AUC_(0～12)分别为(3.416±1.037)μg·mL~(-1)·h 和(3.433±0.910)μg·mL~(-1)·h,AUC_(0～∞)分别为(3.492±1.044)μg·mL~(-1)·h 和(3.523±0.912)μg·mL~(-1)·h。结论:测定方法准确、灵敏、快速,适用于厄多司坦人体药代动力学研究。厄多司坦两制剂主要药代动力学参数无显著性差异,为生物等效制剂。     

Validated HPLC method for determination of amlodipine in human plasma and its application to pharmacokinetic studies

A rapid, simple and sensitive high-performance liquid chromatography (HPLC) method has been developed for quantification of amlodipine in plasma. The assay enables the measurement of amlodipine for therapeutic drug monitoring with a minimum detectable limit of 0.2 ng ml(-1). The method involves simple, one-step extraction procedure and analytical recovery was about 97%. The separation was performed on an analytical 125 x 4.6 mm i.d. Nucleosil C8 column. The wavelength was set at 239 nm. The mobile phase was a mixture of 0.01 M sodium dihydrogen phosphate buffer and acetonitrile (63:37, v/v) adjusted to pH 3.5 at a flow rate of 1.5 ml min(-1). The calibration curve was linear over the concentration range 0.5-16 ng ml(-1). The coefficients of variation for inter-day and intra-day assay were found to be less than 10%.     

HPLC determination of telmisartan in human plasma and its application to a pharmacokinetic study

A sensitive, simple, and accurate HPLC method was developed for the assay of telmisartan in human plasma. Using naproxen as internal standard, the assay involved liquid-liquid extraction of the compound from acidified plasma into organic solvent and reversed-phase chromatography with fluorescence detection. The assay was shown to be linear from 0.5 to 1000 ng/mL. In 24 healthy volunteers, the plasma concentrations of the drug were determined after a single oral dose of 160 mg.