高效液相色谱法测定人血浆中左氧氟沙星浓度

建立测定人血浆中左氧氟沙星浓度的高效液相色谱法,并应用于人体药代动力学研究。血浆样品中加入内标洛美沙星后用乙腈沉淀蛋白,上清液用氮气吹干。色谱柱为Diamonsil C18柱,流动相为0.01mol.L-1磷酸二氢钾缓冲液(含三乙胺0.3%,磷酸调至pH 3.20)?乙腈(83∶17),流速为1.0ml.min-1。紫外检测波长294 nm。血浆中内源性物质对样品测定无干扰。本方法线性范围为0.05~5μg.ml-1(r=0.9991),最低定量浓度为0.05μg.ml-1,提取回收率大于85%,方法回收率为99.7%~103.3%,日内、日间RSD均小于4%。本法简便、准确,适用于左氧氟沙星药代动力学的研究。     

高效液相色谱法测定人血浆中左氧氟沙星的浓度

目的 建立高效液相色谱法测定人血浆中左氧氟沙星血药浓度的方法.方法 采用Diamonsil C18色谱柱,流动相为水(含0.1％甲酸和0.4％三乙胺)-乙腈(14:86),流速为1.0 mL· min-1,紫外检测波长290 nm,柱温为35℃,采用蛋白沉淀法处理血浆样品.结果 左氧氟沙星血浆浓度在0.207～26.47 μg·mL-1(r=0.999 8)线性关系良好;低、中、高3种浓度的平均相对回收率分别为90.0％、98.3％、95.0％;日内和日间精密度RSD均＜10％.结论 本方法简便、快速、准确、灵敏度高,可用于左氧氟沙星血药浓度测定和人体药动学研究.     

高效液相色谱法测定人血浆氟康唑浓度

目的 建立测定人血浆氟康唑浓度的高效液相色谱法。方法 采用Eurosphex 100 C18柱，以乙腈-磷酸二氢钾（KH₂PO₄,0.01 mol·L^-1）(28：72,V/V,用磷酸调节pH值至3.0)为流动相，非那西丁为内标，紫外检测波长为261 nm，测定人血浆氟康唑浓度。结果 血浆氟康唑浓度在0.1～10.0 μg·mL^-1范围内线性关系良好，r＞0.999(n=8)，低、中、高3个浓度(0.25,2.50,9.00 μg·mL^-1)的样品提取回收率分别为104.95%,89.93%和99.20%。结论 所建立的方法操作简便、灵敏度高、重现性好，可用于临床血浆氟康唑浓度测定及人体药动学研究。     

柱切换高效液相色谱法测定血浆左氧氟沙星浓度

目的 应用柱切换高效液相色谱(HPLC)技术直接测定血浆中左氧氟沙星的浓度.方法 采用手动柱切换装置,分析柱采用大连依利特公司的Hypersil ODS C18柱（200 mm×4.6 mm,5 μm）,预柱采用μBondapak C18（50 mm×4.6 mm,37～50 μm,干法自填）.分析流动相（AMP）为甲醇 磷酸二氢钾缓冲液（0.01 mol•L-1,pH值＝2.5） 四丁基溴化铵（0.05 mol•L-1） 三乙胺＝40：60：4：0.2（V/V）;预处理流动相（PMP）为磷酸二氢钾缓冲液（0.01 mol•L^-1,pH值＝2.5） 四丁基溴化铵（0.05 mol•L^-1）＝100：1（V/V）.分析流动相流速1 mL•min^-1,预处理流动相流速2 mL•min^-1.检测波长为294 nm.结果左氧氟沙星在100～8 000 ng•mL^-1内有良好的线性关系.相关系数r＝0.999 8,方法平均相对回收率98.8%,日内及日间差小于10%,最低检测限0.05 μg•mL^-1（S/N≥3）.结论 样品无须预处理,直接进样分析测定,简便易行.     

高效液相色谱法测定人血浆中苦参碱的浓度

目的建立高效液相色谱（HPLC）法测定人血浆中苦参碱的浓度。方法以0．02mol／L磷酸二氢钾溶液（含0．4％三乙胺，以磷酸调节pH值至6.0±0．1）-乙腈（88：12）为流动相，尼扎替丁为内标，血浆样品经二氯甲烷萃取后采用HPLC法测定。结果苦参碱质量浓度的线性范围是0．102～20．4μg／mL，平均相对回收率为93．3％～108，6％，日内和日间精密度RSD均小于10％，苦参碱的最低检测限为25ng／mL。结论该方法快速、准确、灵敏，可用于苦参碱的药代动力学研究。     

高效液相色谱法测定猫血浆利多卡因浓度

目的应用高效液相色谱法测定猫血浆中利多卡因浓度,探索试验方法及精确度,以便进一步应用于利多卡因对心血管系统影响的药理学试验。方法应用高效液相色谱法分别测定对照溶液和猫血浆中利多卡因浓度。结果猫血浆中内源性物质对测定无干扰;浓度在0．43—427．00μmol／L范围内与峰面积线性关系良好;峰面积的日内相对标准偏差（RSD）分别为2．16％、1．48％和0．65％;峰面积的日间RSD分别为3．38％、1．78％和0．76％;绝对回收率分别为（84．25±3．54）％、（82．33±3．87）％和（86．38±1．75）％;方法回收率分别为（99．58±5．43）％、（100．88±4．65）％和（99．54±3．65）％。结论高效液相色谱法稳定、回收率高,并且检测方法简单,适用于大多数的实验室,可应用于药物代谢动力学的研究。     

反相高效液相色谱法测定人体血浆中表阿霉素的含量

采用反相高效液相色谱法(以柔红霉素为内标)测定血浆中表阿霉素的含量,流动相为5mmol/LH3PO4-甲醇-异丙醇-乙晴(6∶9∶7∶2,pH2.9),YWGC18不锈钢色谱柱,荧光检测波长λex=450nm,λem=530nm.血浆中样品经氯仿-甲醇-异丙醇=5∶2∶3抽提液抽提处理后进样测定.血浆中表阿霉素的浓度在0.03～2.4mg/L范围内峰面积与柔红霉素的峰面积之比呈线性关系(r=0.9998),方法对表阿霉素的平均回收率为89%～90.7%.最低检测浓度为0.01mg/L.本法灵敏度高,线性范围大,符合临床用药的血药浓度监测和药代动力学研究的分析方法要求,并用于40例已服用表阿霉素的癌症病人的血浆药物含量的测定.     

Simultaneous determination of Aprepitant and two metabolites in human plasma by high-performance liquid chromatography with tandem mass spectrometric detection

A method for the simultaneous determination of Aprepitant, I (5-[[2(R)-[1(R)-(3,5-bistrifluoromethylphenyl)ethoxy]-3(S)-(4-fluorophenyl) morpholin-4-yl]methyl]-2,4-dihydro-[1,2,4]triazol-3-one) and two active metabolites (II and III) in human plasma has been developed. The method was based on high-performance liquid chromatography (HPLC) with atmospheric pressure chemical ionization tandem mass spectrometric (APCI-MS-MS) detection in positive ionization mode using a heated nebulizer interface. The analytes and internal standard (IV) (Fig. 1) were isolated from basified plasma using liquid–liquid extraction. The organic extracts were dried, reconstituted in mobile phase and injected into the HPLC-MS/MS system.

The analytes were chromatographed on a narrow bore (50 mm×2.0 mm, 3 μm) Keystone Scientific’s Prism R.P. analytical column, with mobile phase consisting of acetonitrile (ACN):water containing trifluoroacetic acid with pH adjusted to 3 (40:60, v/v) pumped at a flow rate of 0.5 ml/min. The MS-MS detection was performed on a Sciex API 3000 tandem mass spectrometer operated in selected reaction monitoring mode. The precursor→product ion combinations of m/z 535→277, 438→180, 452→223 and 503→259 were used to quantify I, II, III, and IV, respectively, after chromatographic separation of the analytes. The assay was validated in the concentration range of 10–5000 ng/ml for I and II and 25–5000 ng/ml for III when 1 ml of plasma was processed. The precision of the assay (expressed as coefficient of variation, CV) was less than 10% at all concentrations within the standard curve range, with adequate assay accuracy. Matrix effect experiments were performed to demonstrate the absence of any significant change in ionization of the analytes when comparing neat standards to analytes in the presence of plasma matrix. This assay was utilized to support a clinical study where multiple oral doses of I were administered to healthy subjects to investigate the pharmacokinetics, safety, and tolerability of Aprepitant. Concentrations of the two most active metabolites, which if present in high concentrations would increase the neurokinin-1 (NK₁) receptor occupancy level and therefore potentially contribute to the antiemetic action of Aprepitant, were determined.     

高效液相色谱法测定人血浆中左布比卡因的浓度

目的建立高效液相色谱法测定人血浆中左布比卡因的浓度。方法以罗哌卡因为内标,色谱柱为Hypersil C_(18)柱(200 mm×4.6 mm,5μm),流动相采用0.01 mol·L~(-1)磷酸二氢钾-乙腈(87:13,V:V,pH=3.4),流速2.0 mL·min~(-1),检测波长为210 nm,柱温40℃。结果标准曲线方程为Y=0.310 1 X+ 0.008 9,r=0.999 7,左布比卡因的质量浓度在0.012 5～2 mg·L~(-1)范围内呈良好的线性关系,最低检测限为0.01 mg·L~(-1);方法回收率在96%～105%之间;日间、日内精密度RSD均<5%。结论本方法可用于临床上左布比卡因血药浓度的监测和药动学研究。     

高效液相色谱双波长法测定人血浆中舒尼替尼的浓度

目的 建立人血浆中舒尼替尼的高效液相色谱测定方法,用于临床进行药物浓度监测.方法 血浆样品经乙酸乙酯乙酯萃取后,采用高效液相色谱法(HPLC)进行分析.XDB-C18柱分离,流动相采用甲醇-0.02 mol/L磷酸二氢钠溶液,流速为1 ml/min;梯度洗脱在0～6 min甲醇-0.02 mol/L磷酸二氢钠溶液为70:30,6.1～15 min甲醇-0.02 mol/L磷酸二氢钠溶液为80∶20;利用光电二极管阵列检测器对流份进行双波长同时检测(舒尼替尼391 nm,内标300 nm),柱温30℃.结果 内源性物质不干扰测定,舒尼替尼的线性范围为0.5～12mg/L(r =0.996),最低定量限为0.5mg/L,基质效应为93.36％～104.26％(n=5),加样回收率为73.12％ ～86.50％ (n =5).结论 建立的HPLC方法简便、灵敏、准确、所需样本量小,可以用于临床血药浓度测定.     

A high-performance liquid chromatographic method for the determination of stobadin pharmacokinetics in serum

A high-performance liquid chromatographic method was developed to determine stobadin pharmacokinetics in dog and man. The relative bioavailability of stobadin dipalmitate compared with dihydrochloride was 46.4 per cent in dog. In man peak serum concentrations ranged from 12 to 289 ng ml-1 after a single oral dose of stobadin dipalmitate (0.79 to 2.5 mgkg-1).     

反相高效液相色谱法测定人血浆中甲磺丁脲的含量

目的建立反相高效液相色谱法用于测定人血浆中甲磺丁脲的含量。方法采用Eclipse XDB-C_(18)色谱柱,以乙腈-25 mmol·L~(-1)乙酸钠缓冲液(pH=3.3,32:68)为流动相,流速1.0 mL·min~(-1),检测波长为229 nm,柱温35℃。血样经等体积比的0.6 mol·L~(-1)三氯乙酸处理后,离心,取上清液20μL,进样检测。结果甲磺丁脲血浆药物浓度在0.5～100 mg·L~(-1)内,线性关系良好(r=0.999 6);回收率为93.0%～105.0%;日内RSD≤3.80%,日间RSD≤6.31%。结论本方法简单快速、准确灵敏、回收率高、重现性好,适用于甲磺丁脲的血药浓度测定。     

Determination of macelignan in rat plasma by high-performance liquid chromatography with ultraviolet detection

A high-performance liquid chromatographic method was developed for the determination of macelignan in rat plasma and applied to the pharmacokinetic study of macelignan in rats. Chromatographic separation was achieved on a conventional ODS column with the mobile phase of water: acetonitrile: methanol = 35:32.5:32.5 (v/v/v %). The flow rate of isocratic elution was 1 mL/min and peaks were detected at 240 nm. The limit of detection was 10 ng/mL and the limit of quantitation was 20 ng/mL. The calibration curve was linear over the concentration range of 50-5000 ng/mL. Intra-and inter-day precision for the assay over the concentration range was below 10 % and the accuracy ranged between 96.0-107% for intra-day and 98.8-114% for inter-day, respectively. The method was applied to the single dose pharmacokinetic study of macelignan in rats and the results showed that this HPLC method was adequate to support the in vivo pharmacokinetic study of macelignan.     

Simple high-performance liquid chromatographic method for the determination of acyclovir in pharmaceuticals

An assay method for the determination of acyclovir from pharmaceutical preparations has been developed for assessment of product quality utilising high-performance liquid chromatography. The chromatographic conditions comprised a reversed-phase C18 column (250 x 4.6 mm i.d.) with a mobile phase of acetonitrile-20 mmol l(-1) aqueous ammonium acetate buffer of pH 4.5 (40:60). The flow rate was 0.8 ml min(-1) and UV detection was used at 250 nm. Calibration graph was linear in the range 1.98-59.4 microg ml(-1). The method has been validated according to current guidelines including assay of pharmacopoeial standard tablets. Recoveries ranged from 96.64 to 99.53%. The exipients present in the tablets did not interfere with the method.     

高效液相色谱法测定血浆中氟哌啶醇浓度

目的：建立高效液相色谱法测定血浆中氟哌啶醇浓度的方法。方法：以乙腈甲醇０ ．０２５ｍｏｌ／Ｌ 磷酸二氢钾（４５∶５∶５０ ,ｖ／ｖ） 为流动相,氯氟哌啶醇作内标,紫外波长２４８ｎｍ 处检测。结果：血浆中氟哌啶醇的最低检测浓度为０ ．５ｎｇ／ｍｌ,平均提取回收率为８６ ．６ ％ ±４ ．９ ％ ,线性范围１ ～５０ｎｇ／ｍｌ（ｒ ＝ ０ ．９９９８） ,日内和日间ＲＳＤ 分别小于８ ％ 和９ ％ 。结论：方法灵敏、快速、准确,可满足临床治疗药物的监测工作