Determination of Thiamphenicol in Serum and Cerebrospinal Fluid with High-Pressure Liquid Chromatography

Abstract

A procedure for quantitation of thiamphenicol in serum and cerebrospinal fluid was developed using high-pressure liquid chromatography. The drug was extracted from biological samples with methanol and separated by reverse-phase high-pressure liquid chromatography. Detection and subsequent quantitation were performed at 254 nm by on-line ultraviolet spectrophotometry. After the intramuscular administration of a single dose of 1 g of thiamphenicol to a patient, a poor transmission of the drug across the hematoencephalic barrier was demonstrated by this assay.     

Measurement of Cefixime in Serum and Cerebrospinal Fluid by High-Performance Liquid Chromatography

Abstract

Cefixime is a new cephalosporin antibiotic for oral administration. A high-performance liquid chromatographic (HPLC) method was developed to measure cefixime in small volumes of serum and cerebrospinal fluid (CSF) to conduct a pharmacokinetics study in pediatric patients. The assay involved precipitation of serum proteins with 6% trichloroacetic acid, using 7-hydroxycoumarin as an internal standard. Chromatographic separation was accomplished using ultrasphere C8 column and mobile phase containing 15% acetonitrile in a buffer at a detection wave length of 280 nm. The retention time of cefixime and 7-hydroxycoumarin was about 5 and 9 minutes, respectively. The method was suitable for quantitation of cefixime at a concentration ranging from 0.05 to 10 μg/ml. The coefficient of variation was less than 3%. The technique was used successfully to measure cefixime in serum and CSF obtained from an infant receiving cefixime.     

RP-HPLC测定兔血清和脑脊液中甲硝唑含量

报告了用RP-HPLC测定免血清和脑脊液中甲硝唑浓度的方法，采用ZorbaxC8柱，NaH2PO4水溶液（0.0075mol／L）-甲醇（4:1，PH4.0）为流动相，氢氯噻嗪为内标，检测波长320um。线性范围0.5～80mg／L，最低检出浓度80μg／L（信噪比为3）。     

反相高效液相色谱法测定实验动物血液和脑组织中川芎嗪

 用反相高效液相色谱法测定了川芎药材、实验动 物血液和脑匀浆中的川芎嗪,方法简便快速。在270 nm检测波长下,不经浓缩可检测动物体 内1 mg/L的川芎嗪,川芎嗪在5～500 mg/L范围内具有良好的线性关系,线性相关系数为0.99 9。川芎嗪的加标回收率为98%～103％。川芎提取物样品、处理后的动物血清和脑匀浆样品具 有较好的稳定性,室温下可放置1星期。     

Determination of Piperacillin in Plasma and Cerebrospinal Fluid by High Performance Liquid Chromatography

Abstract

Reversed-phase high performance liquid chromatography was applied to the quantitative determination of a new β lactam antibiotic piperacillin. The procedure was applied to human plasma and cerebrospinal fluid samples. After an extraction of plasmaor cerebrospinal fluid by dimethyl formamide, chromatographic separation was effected on a bonded hydrophobic stationary phase with one mobile ohase: methanol-phosphate buffer. This assay was applied to study human pharmacokinetics on ten patients with purulent meningitis during their therapy. Simultaneous determination of piperacillin in plasma and cerebrospinal fluid one and two hours after piperacillin perfusion showed a good penetration of this antibiotic in human cerebrospinal fluid.     

反相高效液相色谱法测定川芎饮片、实验大鼠血清和脑匀浆中的阿魏酸

 用反相高效液相色谱法测定了川芎饮片、实验大鼠血清和脑匀浆中的阿魏酸。分离柱为Nova Pak C18(3 9mmi.d .× 15 0mm) ,流动相为甲醇 水 乙酸 (体积比为 35∶6 5∶0 5 ) ,在 32 0nm波长下检测 ,用外标法定量。阿魏酸在 0 85mg/L～ 4 0 0mg/L范围内有良好的线性关系 ,线性相关系数为0 9990 4。阿魏酸的加标回收率为 95 %～ 10 2 %。     

气相色谱法测定线粒体脑肌病患者血清和脑脊液中的乳酸

血清和脑脊液样品经甲酯化处理,氯仿提取,氮气吹干,残留物用庚烷溶解后进样,用气相色谱法测定线粒体脑肌病患者血清和脑脊液中乳酸含量。结果显示, 线粒体脑肌病患者的血清、脑脊液中乳酸含量分别为(294±101) mg/L 和(312±103) mg/L,比正常人((192±37) mg/L 和(153±81) mg/L)以及神经系统其他疾病患者((150±34) mg/L和(173±29) mg/L)显著增高(P＜0.05)。该方法可作为筛选线粒体脑肌病的临床诊断方法。     

反相高效液相色谱法快速测定7种四环素类抗生素

建立了一种反相高效液相色谱梯度洗脱分离测定四环素类药物的新方法。采用DiamonsilTM C1 8ODS(2 5 0mm× 4 .6mmi.d ,5 μm)色谱柱 ,以甲醇 乙腈 0 .0 1mol/L草酸为流动相 ,流速 1.0mL/min ,2 70nm检测 ,在10min内分离检测四环素等 7种化合物。同时还研究了流动相组成、梯度条件、pH值、草酸浓度等因素对分离效果的影响。     

高效液相色谱法测定人血清中假尿嘧啶核苷的浓度

应用反相高效液相色谱法测定人血清中假尿苷（ＰＤ）的含量,色谱柱为Ｎｏｖａ－ＰａｋＣ１８３．９ｍｍ×１５０ｍｍ,流动相为０．０４ｍｏｌ／Ｌ磷酸二氢钾缓冲液（ｐＨ４．０）,检测波长为２６３ｎｍ,线性范围为０．７～６．８μｍｏｌ／Ｌ,回收率为９３．５０％,日间误差ＣＶ＝３．１１％（ｎ＝６）。同时测定了部队体检正常人血清中ＰＤ的浓度,并用于临床观察肝炎、肾病、肺癌等多种疾病以及Ｈｅ－Ｎｅ激光治疗前后患者血中ＰＤ含量的变化。正常人血中ＰＤ的浓度无性别差异,成年人的正常值与文献一致。     

液相色谱法快速测定化妆品中抗氧化剂

本文提出了一种应用高效液相色谱法同时测定化妆品中三种常用抗氧化剂的快速方法。应用微量化学法技术处理样品，提高了分析速度。样品用乙腈提取，提取液过Ｃ１８微柱净化。净化液在反相色谱柱上进行测定，检测波长２８０ｎｍ，流动相为２０％乙腈水溶注，１０ｍｉｎ内线性梯度变为１００％乙腈，乙腈水均各加５％醋酸。     

用高效液相色谱法快速测定甜菊糖甙

本文介绍了用高效液相色谱法分离测定甜菊糖甙的四种成分,测定了各成分的相对百分含量及甜菊饮料制品中各糖甙成分及糖类的含量,并做了精密度和回收率的验证。该法简便快速,效果良好。色谱条件为:μ-Bondapak NH_2往,柱前加Bondapak AX/Corasil预柱;乙腈:0.02M(NH_4))2 HPO_4水溶液=75:25作流动相,流速为2.0ml·min~(-1);示差折光检测。     

Determination of Acyclovir in Human Serum by High-Performance Liquid Chromatography

Abstract

A method was developed for determination of concentrations of acyclovir in serum. Serum proteins were precipitated with equal part of 5% perchloric acid. High-performance liquid chromatography was used for separation from endogenous compounds and detection was done with spectrophotometry. The assay is simple and precise and seems well suited for pharmacokinetic studies.     

高效液相色谱法快速检测氨基葡萄糖含量

应用高效液相色谱法,建立了硫酸氨基葡萄糖氯化钾胶囊中氨基葡萄糖含量的快速测定方法。采用Hedera NH2色谱柱（250 mm ×4.6 mm,5 μm）,流动相为乙腈-磷酸缓冲液（ 65∶35）,流速为 1.0 mL/min,可变波长紫外检测器,检测波长为195 nm。 结果表明,在上述色谱条件下,氨基葡萄糖浓度在1.6~2.4 g/L范围内线性关系良好,检出限为7.81 mg/L,精密度（RSD,n=6）为0.53%;平均加标回收率为 100%,相对标准偏差为1.1%。该法准确、可靠,无需衍生反应,适用于硫酸氨基葡萄糖氯化钾胶囊中氨基葡萄糖的含量测定。     

反相高效液相法测定血清中的佐匹克隆

 建立了测定血清中佐匹克隆的反相高效液相法 (外标法 )。血样用正丁基氯提取后进行分离。采用的柱为LiChroCART 12 5 4柱 (LiChrospher 6 0RPselectB填料 ,5 μm ,12 5mm× 4mmi d ) ,流动相为乙腈 0 0 2mol/LKH2 PO4缓冲溶液 (体积比为 2 0∶80 ) ,紫外检测波长为 2 5 4nm。当佐匹克隆在血清中的添加质量浓度分别为 4 0 0 μg/L ,16 0 0 μg/L和6 4 0 0 μg/L时 ,血清中佐匹克隆的回收率分别是 (73 4± 3 2 ) % ,(82 2± 4 1) %和(90 3± 4 5 ) %。方法的最低检出限为 15 μg/L。方法适用于法庭毒物分析 ,简便、快速。     

高效液相色谱法测定血清中茶碱浓度

采用高效液相色谱,分析柱：３μｍ,３．３ｃｍ＊４．６ｍｍ,Ｉ．Ｄ（Ｐｅｒｋｉｎ Ｅｌｍｅｒ,ＵＳＡ）;预柱：１０μｍ,１ｃｍ＊２．１ｍｍ,Ｉ．Ｄ（Ｐｅｒｋｉｎ ＥＬｍｅｒ,ＵＳＡ）;以乙酰氨基酚为内标对氯仿－异丙醇（９５：５,Ｖ／Ｖ）提取样品进行了分析,流动相：０．１ｍｏｌ／Ｌ醋酸缓冲液（ＰＨ＝４．５）－甲醇（７０：３０,Ｖ／Ｖ）;检测波长：２７０ｎｍ;流速０．５ｍＬ／ｍｉｎ,３ｍｉｎ即完成一次茶     

Determination of Serum Chloramphenicol by High Performance Liquid Chromatography

Abstract

A simple single extraction procedure for the analysis of serum chloramphenicol levels by high performance liquid chromatography (HPLC) is described. Serum is mixed with buffer and extracted with ether, which is then evaporated. The residue is dissolved in the eluting solvent and analyzed on a reverse-phase column. The eluting solvent is methanol/distilled water (50/50, V/V) and the effluent is monitored at 280 nm. Serum samples as small as 50 μl can be used.     

液相微萃取-高效液相色谱法快速测定唾液中尼古丁含量

建立了一种以液相微萃取为样品前处理技术,结合高效液相色谱快速、有效测定唾液中尼古丁含量的方法。确定了以磷酸三丁酯为有机溶剂、2 mL 0.05 mol/L KOH调节2 mL样品溶液为给出相,10 mmol/LKH2PO4(pH=3.0)为接收相;搅拌速率为500 r/min,萃取时间为17 min的尼古丁优化萃取条件。方法的线性范围0.1-50 mg/L,相关系数r2=0.9996;检出限为0.05 mg/L(S/N=3);相对标准偏差<5%(n=5);相对回收率为96.3%-102.2%。实验证明该法可用于唾液等生物体液中碱性物质的测定。     

高效液相色谱对液态奶中三聚氰胺的快速测定

建立了有机溶剂提取和离子对色谱相结合的三聚氰胺快速检测方法.样品中加入有机溶剂振荡提取,取上清液过滤进行高效液相色谱(HPLC)分析.对丙酮、乙腈、乙醇和异丙醇的提取物分别在甲醇-离子对试剂流动相体系和乙腈-离子对试剂流动相体系中进行测定和比较.结果显示,选择合适的流动相,使用丙酮、乙醇或异丙醇为提取剂可以获得较好的提取效果.在甲醇-离子对试剂流动相体系中,三聚氰胺的质量浓度在1.0 ～100.0 mg/L范围内与色谱峰面积呈良好的线性关系(r=0.999 98),检出限为0.1 mg/kg,采用丙酮为提取剂,加标回收率为97% ～103%,相对标准偏差(RSD)小于5%.     

Analysis of 3-Methoxy-4-Hydroxyphenylglycol in Human Cerebrospinal Fluid by Gas Chromatography Mass Spectrometry and Electrochemical Detection Liquid Chromatography

Abstract

Gas chromatography mass spectrometry [GCMS] and liquid chromatography with electrochemical detection [LCEC] have been compared in simultaneous determination of 3-methoxy-4-hydroxy-phenylglycol [MHPG] in human cerebrospinal fluid [CSF]. Both free and sulphate conjugated MHPG have been measured in these samples. By Spearman Rank Correlation non-parametric analysis both instrumental techniques related significantly for all quantitated samples.     

对小鼠血清中乳梨醇含量的测定

建立了测定小鼠血清中乳梨醇的含量的高效液相色谱法。分析柱为ＷａｔｅｒｓＳｕｇａｒ－Ｐａｋｌ（钙型）柱,流动相为重蒸水,柱温９０℃,采用示差折光检测器检测定量。回收率为９８．６％,方法的最低检测限为０．１μｇ（Ｓ／Ｎ＝３．７５）,在０～６００ｍｇ／Ｌ的范围内呈良好的线性关系,ｒ＝０．９９９２,日内和日间ＲＳＤ均小于１．０％（ｎ＝５）。