高效液相色谱法测定司巴沙星血药浓度

建立血清中司巴沙星浓度的HPLC测定法。方法：0.02mol／L磷酸二氢钾-乙腈(70：30),内含0.1％二乙胺,磷酸调pH3.0为流动相,替硝唑为内标,检测波长298nm,最低检测浓度为0.005mg／L。采用Shimpack-CLC ODS C₁₈柱(150mm×6mm,5μm),加YGW C₁₈预柱。结果：选择浓度0.2,0.8和1.6mg／L,回收率分别为95.92％,99.87％,和97.90％,日内RSD分别为9.04％,8.05％和3.45％,日间RSD分别为1.08％,3.86％和1.36％。结论：本法快速、简便、准确性好,灵敏度高。适用于药动学、药效学及药物相互作用方面的研究。     

高效液相色谱法测定司巴沙星片临床血药浓度

建立测定人血浆中司巴沙星药物浓度的ＲＰ－ＨＰＬＣ法,为临床合理用药提供必要的分析方法。方法：采用ＨＰＬＣ法,色谱柱为ＹＷＧ ＲＰ－Ｃ１８（１５０ｍｍ＊４．６ｍｍ,１０μｍ）;流动相为５０ｍｍｏｌ／ＬＮａＡｃ－ＨＡｃ缓冲液（ｐＨ５．０）;乙腈：甲醇＝７０：２０：１０（含０．０４％三乙胺,调ＰＨ２．４０）,检测波长２９９ｎｍ。血样（含内标对羟基苯乙酮）用７ｍｌ二氯甲烷一次提取,浓缩后取２０μｌ进样作Ｈ     

高效液相色谱法测定克林沙星血药浓度

目的 :建立用高效液相色谱法测定血浆中克林沙星浓度的方法。方法 :血浆样品在酸性条件下 ,以Oasis小柱提取环丙沙星为内标 ,采用LichrosorbC18(5 μm)柱 ,流动相为乙腈 - 0 0 5mol·L-1柠檬酸三乙胺溶液 (pH 2 5 ) (2 0∶80 ) ,流速为 1 0mL·min-1,检测波长 30 0nm ,克林沙星和内标的保留时间分别为 7 1min和 4 5min。结果 :线性范围在 0 0 3～10 μg·mL-1(r=0 9998) ,最低检测浓度为 0 0 2 μg·mL-1,RSD <7%。用本法测定了 6只大鼠灌胃剂量 5 0mg·kg-1克林沙星后血浆中克林沙星的浓度经时变化过程。结论 :本方法可用于克林沙星的血药浓度测定及药代动力学研究。     

高效液相色谱法测定人血清中司帕沙星药物浓度

目的建立测定人血浆中司帕沙星药物浓度的方法。方法采用二氯甲烷萃取，高效液相色谱法测定。色谱柱：GeminiC18（250mm×4．6mm，5μml流动相：0．01mol·L^-1，磷酸二氢钾-三乙胺（磷酸调PH=3．0）-甲醇（34．8：0．2：65）；流速：1．2mL·min^-1；紫外检测器：波长292nm，柱温30℃。结果司帕沙星的保留时间为9．6min，定量线性范围：0．016。2．000μg·ml^-1，方法回收率〉90％（n=5），日内、日间RSD〈10％（n=5）。结论本方法快速，定量准确，可用于血药浓度测定及人体药代动力学研究。     

反相高效液相色谱法测定格拉司琼血药浓度

目的 :建立格拉司琼血药浓度的反相高效液相色谱测定方法。方法 :以甲醇 0 .0 5mol·L-1醋酸钠缓冲液 (pH6 .0 ,含0 .2 5 %三乙胺 ) (83∶17)为流动相 ,激发波长为 30 5nm ,发射波长 36 5nm ,血浆样品采用乙酸乙酯提取后进样。结果 :格拉司琼在0 .2～ 15 μg·L-1浓度范围内线性关系良好 ,平均回收率 (98.6± 7.4) % ,日内RSD≤ 4.9% ,日间RSD≤ 8.5 %。结论 :方法简便 ,准确 ,灵敏 ,可用于格拉司琼血药浓度测定。     

高效液相色谱法测定人血浆中司帕沙星药物浓度

目的建立测定人血浆中司帕沙星的药物浓度的方法。方法采用乙腈萃取,高效液相色谱法测定。色谱柱:Hypersil BDS-C18(4.6 mm×150 mm,5μm);流动相:0.25%磷酸乙腈溶液(450∶100,用三乙胺调pH=2.50);流速:1 mL/min;紫外检测器:波长298 nm,柱温40℃。结果司帕沙星的保留时间为6.1 min,定量线性范围:0.06~2.16μg/mL,方法回收率>90%(n=5),日内、日间RSD<10%(n=5)。结论本方法快速,定量准确,可用于血药浓度测定及人体药代动力学研究。     

反相高效液相色谱法测定卡德沙星在健康人体的血药浓度

目的 建立反相高效液相色谱法测定人血浆中卡德沙星(喹诺酮类抗菌药)浓度的方法.方法 以加替沙星为内标,血浆样品经6%高氯酸沉淀,梯度洗脱,检测波长286 nm.结果 卡德沙星在0.1～10.0 mg·L-1内线性关系良好,相对回收率为96.41%～109.52%,日内、日间RSD均小于15%;在2名中国健康受试者3 h恒速静滴卡德沙星400 mg后,其药代动力学符合开放二房室模型,主要药代动力学参数:Cmax=3.42、6.04 mg·L-1,t1/2β=7.74、6.73 h,AUC0-t=32.35、28.26 mg·h·L-1.结论 此方法准确、灵敏度高、专属性强,适用于临床药代动力学研究.     

高效液相色谱法测定格拉司琼的血药浓度

目的：建立人血浆中格拉司琼浓度的测定方法。方法：采用ＨＰＬＣ法,荧光检测器,色谱柱为Ｃ８柱（４．６ｍｍ×１５０ｍｍ,５μｍ）;流动相为乙腈－０．１ｍｏｌ／Ｌ醋酸钠ｐＨ ４．７（２５∶７５, ｖ／ｖ）,内含１０ｍｍｏｌ／Ｌ己烷磺酸钠;荧光检测波长：Ｅｘ＝３０５ｎｍ、Ｅｍ＝３６０ｎｍ。血液样品用甲苯一次提取,吹干后残渣用流动相复溶,２０μｌ进样。结果：格拉司琼血药浓度标准曲线在０．１５６～４０ｎｇ／ｍｌ间呈线性相关,Ｙ＝５．６０７２ Ｘ—１４３７ ２（ｒ＝０．９９３ ３．ｒＳＮ＝３）。呈低检测限为０．１５６ ｎｇ／ｍｌ。方法的平均回收率为１０４．２％;日内及日间精密度均小于１０％。结论：本方法具有简便、灵敏、准确等优点,为该药物的监测与临床药理研究提供了分析方法。     

A high-performance liquid chromatographic assay for sparfloxacin

A specific and sensitive high-performance liquid chromatographic procedure was developed for the assay of sparfloxacin in raw material and tablets. It was also found that the excipients in the commercial tablet preparation did not interfere with the assay. The method validation yielded good results and included the range, linearity, precision, accuracy, specificity and recovery. This method can also be applied to stability studies.     

High-performance liquid chromatography assay for moxifloxacin: pharmacokinetics in human plasma

A sensitive high-performance liquid chromatographic (HPLC) method for the determination of moxifloxacin in human plasma using fluorescence detection was developed. The drug and an internal standard (norfloxacin) were subjected to precolumn derivatization with 4-chloro-7-nitrobenzodioxazole (NBD-CI). The chromatographic separation was achieved by HPLC using a mixture of acetonitrile-10 mM orthophosphoric acid (pH 2.5) (80:20, v/v) as the mobile phase with isocratically system, a C18 column. The derivative is highly fluorescent at 537 nm, being excited at 464 nm. The linear and reproducible calibration curve over the range was 15-2700 ng/mL of moxifloxacin in human plasma. The limits of detection and quantitation were 6 and 15 ng/mL, respectively. This method was applied in pharmacokinetic studies moxifloxacin preparations in healthy volunteers.     

Sensitive liquid chromatography assay for the determination of amikacin in human plasma

A selective LC method with on-line post-column derivatization is described for the determination of amikacin in biological fluids. Chromatography was performed on a reversed-phase column, using pentane sulphonic acid as an ion-pairing reagent. For the analysis of biological fluids, amikacin and the internal standard tobramycin were extracted using an ion exchanger (Sephadex). Following complete removal of plasma proteins, the aminoglycosides were eluted with alkaline sodium sulphate solution and injected into the chromatograph. After chromatographic separation the eluent was mixed with the derivatization reagent (o-phthalaldehyde and mercaptoethanol in borate buffer pH 10.4) in a reaction coil at 50 degrees C. Detection was performed by fluorescence (excitation: 340 nm, emission: 418 nm). The overall run time was 8 min, at a flow rate of 1.2 ml min-1. The limit of quantification was 25 ng ml-1 for amikacin in plasma.     

A high performance liquid chromatography method for simultaneous determination of albendazole metabolites in human serum

A simple assay for albendazole (ABZ) main metabolites-albendazole sulphoxide (ABZ-SO), albendazole sulphone (ABZ-SO(2)) and albendazole amino sulphone (ABZ-SO(2)-NH(2))-in serum using high performance liquid chromatography was developed. The method involves liquid-liquid extraction of the serum by ethyl acetate, clean up with n-hexane and re-extraction with ethyl acetate, followed by separation on RP-C(8) column with a mixture of methanol: acetonitrile: acetic acid: water (40:1:10:49) as the eluting solvent. ABZ-SO and mebendazole-used as internal standard-were detected by UV (lambda=286 nm), and ABZ-SO(2) and ABZ-SO(2)-NH(2) with fluorescence spectrophotometer at (Excitation=286 nm, Emission=333 nm) and (Excitation=286 nm, Emission=315 nm), respectively. The assay was accurate and reproducible with a detection limit of 10 ng/ml for ABZ-SO, 2 ng/ml for ABZ-SO(2) and 4 ng/ml for ABZ-SO(2)-NH(2). Disregarding ABZ determination, which is not of pharmacokinetic importance as it is not found in human plasma after oral administration, the proposed method is appropriate for further pharmacokinetic and metabolism study of this drug.     

高效液相色谱法测定血浆中咪达唑仑浓度

目的 :建立测定血浆中咪达唑仑浓度的反相高效液相色谱法。方法 :以地西泮为内标 ,采用C18柱及保护柱 ;流动相为甲醇 -水 (6 0∶4 0 ,V/V) ,含乙腈 1%、二乙胺 0 1%、磷酸 0 0 5 % ;流速为 0 6mL·min-1;提取液为乙醚 ;采用紫外检测 ,检测波长为 2 2 5nm。结果 :咪达唑仑与内标分离良好 ,保留时间分别为 (11 2 1± 0 5 8)min和 (9 4 1± 0 39)min ;咪达唑仑在 0 1～ 2 0 μg·mL-1范围内线性良好 ,回归方程为Y =9× 10 -4X - 9 17× 10 -2 ,r=0 9998;日内及日间变异均 <6 % ;最低检测浓度 0 0 5 μg·mL-1。结论 :本方法适用于咪达唑仑的药动学和药效学研究     

Determination of ketorolac in human serum by high-performance liquid chromatography

A high-performance liquid chromatographic (HPLC) assay has been developed for the determination of ketorolac in human serum using a new extraction method with a good recovery. Human serum samples (1.0 ml) spiked with known concentrations of ketorolac tromethamine and 10 μg of ketoprofen as the internal standard (IS) were acidified with 200 μl of 1N HCl and extracted with 7 ml ofn-hexane-ether (7∶3 v/v). Extracts were centrifuged and organic layer was back-extracted with 400 μl of 0.1% tromethamine solution. Twenty μl of centrifuged aqueous layer was injected onto a reversed-phase octyl column and eluted with a mixture of acetonitrile, water, methanol, and triethylamine [35∶55∶10∶0.1 (v/v), pH 3.0] at a flow rate of 1.0 ml/min. Ultraviolet detection of ketorolac and IS was carried out at 300 nm. The calibration curve obtained using peak area ratios showed a good linearity (in concentration range 10–150 ng/ml r²=0.9944; in range 50–2000 ng/ml, r²=0.9998). The mean intra-day accuracy and precision for this HPLC method were found to be 3.6 and 3.7%, respectively. The mean inter-day accuracy and precision were found to be 4.0 and 3.7%, respectively, in the concentration range 50–2000 ng/ml. The recovery of ketorolac from serum was 92.0 (±5.7)% at the concentration of 100 ng/ml. This method proved to be readily applicable to the assay of ketorolac in human serum.     

Assay of ertapenem in human serum by high-performance liquid chromatography

Ertapenem is a new carbapenem with a broad spectrum of activity and an extended half-life, permitting once daily administration. Although high-performance liquid chromatography (HPLC) methods have been described for ertapenem, these are complex and involve column switching and thus this type of assay may not suitable for use in routine clinical microbiology laboratories. In this study we report a rapid, straightforward HPLC method for the detection of ertapenem in human serum.     

胶束液相色谱法测定血清中硝苯地平的含量

目的：建立胶束色谱法测定人血清中硝苯地平含量的分析方法。方法：用C18反相色谱法,以甲醇-水-十二烷基硫酸钠（SDS）为流动相（甲醇：水=60：40,内含20mmol.L^_1的SDS）,以峰面积计算含量。结果：方法的回收率为93.98%-100.88%,日内偏差0.91%-1.83%,线性范围0.4-4ug.ml^-1(r=0.9999)。结论：本法舍弃了通常用HPLC法测定血药浓度时血样需预处理这一繁琐步骤,血样可不经分离直接测定。本法操作简便,易行。方法准确、重现性好。     

A simple fluorescence high-performance liquid chromatographic assay for dihydroquinidine in serum

A simple and rapid reversed-phase C-18 high-performance liquid chromatography (HPLC) assay without a prior extraction step for dihydroquinidine (HQD) in serum is described. The method is selective and useful for monitoring HQD and its presumed metabolites, quinidine (QD), N-oxide QD, 3-hydroxy QD (3-OHQD), and 10-11-diol QD. The detection limit for HQD was 0.2 +/- 0.1 mg/L, and the peak heights--concentration curve was linear between 0.5 and 10.0 mg/L. The coefficients of variation within and between runs were identical, 5.0 +/- 1.5%. A 100 +/- 2.5% recovery was obtained by direct injection into the chromatograph of the supernatant following acetonitrile protein precipitation. The total assay time was less than 15 min.     

Fully automated assay for the determination of sumatriptan in human serum using solid-phase extraction and high-performance liquid chromatography with electrochemical detection

A method is described for a fully automated, sensitive, accurate and precise assay for the determination of sumatriptan in human serum. The assay consists of solid-phase extraction followed by reversed-phase HPLC with electrochemical detection. The extraction procedure has been fully automated on a Zymate XP robot linked on-line to the HPLC system. The assay is linear over the analytical range 1–30 ng ml⁻¹ and selective for sumatriptan with respect to endogenous plasma components and GR49336, the major circulating metabolite. The intra-assay data demonstrate a maximum bias and precision across the calibration range of 10% and 6.6%, respectively. The inter-assay data demonstrate a maximum bias and precision across the calibration range of 6.7% and 8.8%, respectively. The extraction efficiency of the assay is approximately 90% and is constant across the calibration range. The assay was used for the determination of sumatriptan in serum clinical samples and was shown to be robust in sustained use over several months. The use of a Zymate XP robot allowed complete automation of the assay, which resulted in high-quality, high-throughput analyses.