反相高效液相色谱法测定人血浆中曲尼司特浓度

报道了用反相高效液相色谱法测定人血浆中曲尼司特浓度。以甲醇－磷酸二氢钾缓冲液（６０∶４０，Ｖ／Ｖ；ｐＨ４．２）为流动相，色谱柱采用ＹＷＧ－Ｃ１８不锈钢柱，紫外３３３ｎｍ波长检测，血浆样品经甲醇沉淀蛋白后直接进样测定。血浆浓度在０．６５～４０ｍｇ／Ｌ范围内线性良好，方法的平均回收率为１００．０％±４．１％。血浆最低检测浓度为０．２ｍｇ／Ｌ。对１０名健康志愿者口服２００ｍｇ曲尼司特后不同时间的血药浓度进行了测定。     

液相色谱法测定血浆中三环类抗忧郁药物

用高效液相色谱法测定了血浆中４种三环类抗忧郁药物：卡马西平、氯氮平、多虑平和阿米替林。方法采用Ｃ_（１８）色谱柱分离,二极管阵列检测器检测,流动相为甲醇：０．５ｍｏｌ／Ｌ三乙胺－０．５ｍｏｌ／Ｌ冰醋酸的水溶液（９０：１０,Ｖ／Ｖ;ｐＨ７．５）。标准曲线的线性范围为０～１０ｍｇ／Ｌ,相关系数在０．９９以上。方法的最小检出浓度为１０～４０μｇ／Ｌ血浆。血中药物经溶剂萃取后,药物的回收率为７３．６７％～９８．２４％,血中杂质不影响药物的检测。方法简便、快速,适用于临床中毒样品的分析。     

高效液相色谱法测定大蒜及其制品中的大蒜素

采用人工合成的大蒜素做为标准品，建立了高效液相色谱法直接测定大蒜及其制品中的大蒜素含量的方法。使用Ｓｐｈｃｒｉｓｏｂ　ＯＤＳ２色谱柱，流动相为甲醇＋水＝６０＋４０，检测波长２５４ｎｍ，进样体积２５μＬ。大蒜素最小检测量为 ２．０ ｍｇ／Ｌ，相对标准偏差为２．８％，回收率为９０．４％～１０３．０％，线性范围为 ０～１２０ｍｇ／Ｌ     

高效液相色谱法同时测定牛肉及其制品中敌草隆、绿麦隆的残留量

介绍了用高效液相色谱同时测定牛肉及其制品中脲类除草剂——敌草隆、绿麦隆残留量的方法。色谱柱为ＳｅｌｅｃｔｏｓｉｌＣ１８柱,流动相为甲醇－水（６０∶４０,Ｖ／Ｖ）,ＵＶ－２４５ｎｍ检测。最小检测量：敌草隆为０．４ｎｇ,绿麦隆为０．５ｎｇ。线性范围均为０．０５～１０ｍｇ／Ｌ。回收率：敌草隆为８７．３４％～８７．６４％,绿麦隆为８８．７８％～９１．９４％。     

碘的凝胶色谱测定方法

建立了碘折凝胶色谱测定方法。色谱条件为：Ｓｈｉｍ－ｐａｃｋ ＤＩＯＬ－１５０柱；流动相甲醇０．０１ｍｏｌ／Ｌ Ｈ３ＰＯ４（１０：９０）流速为１．２ｍＬ／ｍｉｎ；柱温为３５℃，检测波长为２２４ｎｍ；线性范围是０．０１０－１．０ｍｇ／Ｌ，相关系数为０．９９９３，检测限为０．００１ｍｇ／Ｌ，相对标准偏差为１．２％－４．６％；回收率为９１％－９８％。所建立的方法已用于食盐，尿，系带等样品的测试，均取得较好     

铜（Ⅰ）—苯骈三氮唑络合吸附波的极谱研究与应用

本文在０．６ｍｏｌ／Ｌ ＮＨ３－ＮＨ４Ｃｌ缓冲溶液（ｐＨ＝９．８）中，Ｃｕ（Ⅱ）在滴汞电极上还原生成Ｃｕ（Ⅰ），可与苯骈三氮唑（ＢＴＡ）络合，产生一灵敏的络合吸附波，Ｅｐ＝－０．７３Ｖ（ｕｓ，ＳＣＥ）。苯骈三氮唑的浓度在０．４０－１０．０ｍｇ／Ｌ范围内与极谱波峰高呈线性关系，检测下限为０．４０ｍｇ／Ｌ，相对标准偏差为１．４％－３．２％；回收率为９７．５％－１０１．５％。     

反相高效液相色谱法测定雷公藤提取物中雷公藤甲素含量

应用反相高效液相色谱法检测了雷公藤提取物中雷公藤甲素的含量。样品经洗脱提取后,以Ｃ１８化学键合硅胶为固定相,乙腈－水（４０∶６０,Ｖ／Ｖ）为流动相,用２１０ｎｍ波长定量检测。测定结果表明,雷公藤甲素浓度在０．２５～４．００ｍｇ／Ｌ范围内线性良好,最低进样检测浓度为０．１ｍｇ／Ｌ。批内（ｎ＝５）及批间（ｎ＝５）测定相对标准偏差分别为１．９％～６．５％和２．７％～７．８％,回收率为８９．８％～９２．０％。     

高效液相色谱法测定小鼠脑组织单胺递质及其相关化合物

采用苯基柱等度洗脱分离,自然荧光检测法,直接测定小鼠脑组织匀浆中单胺递质及其相关化合物。优化出了最佳色谱条件,流动相为２０ｍｍｏｌ／Ｌ柠檬酸三钠（ｐＨ４．５０）－甲醇（９５：５,Ｖ／Ｖ）;柱温为３５℃。该方法能同时检测８种化合物。最低检测限为１．０－２．５μｇ／Ｌ,回收率均在９３５以上;线性范围为１．０μｇ／Ｌ－１．０ｍｇ／Ｌ。     

高效液相色谱法测定非诺贝特含量

以甲醇－水（９５：５,Ｖ／Ｖ）为流动相,用ＯＤＳ柱以高效液相色谱法测定非诺贝特含量。紫外检测波长为２８６ｎｍ。非诺贝特在浓度为０．０４－０．２０ｇ／Ｌ间线线性关系良好。重复进样ＲＳＤ＝０．１４％,最低检出浓度为０．１０ｍｇ／Ｌ,平均回收率为９９．６６％。     

多联吡啶螯合物反相高效液相色谱法分离测定铜(Ⅱ)、钴(Ⅱ)、汞(Ⅱ)

以三联吡啶衍生物６，６”－二甲基－４＇－苯基－２，２＇：６＇，２”－三联吡啶（ＴＰＹ）作柱前显色剂，于ＡｃｃＱ－Ｔａｇ柱上，用内含２．０×１０～（－６）ｍｏｌ／Ｌ ＴＰＹ和０．６ ｍｏｌ／Ｌ　ＮａＡｃ－ＨＡｃ缓冲溶液（ｐＨ＝３．５）的甲醇－水溶液（５５：４５，Ｖ／Ｖ）作流动相，流速为１．０ ｍＬ／ｍｉｎ，并以紫外－可见检测器于３１０ｎｍ处进行检测，开发了一种 ＲＰ－ＨＰＬＣ法同时分离测定铜（Ⅱ）、钴（Ⅱ）、汞（Ⅱ）的方法。该方法简便快速，灵敏度高，对于铜、钴、汞的检测限分别是０．００２０、０．００５５和０．００４０ｍｇ／Ｌ。用于实际样品测定，结果满意。     

Quantitative determination of paroxetine and its 4-hydroxy-3-methoxy metabolite in plasma by high-performance liquid chromatography/electrospray ion trap mass spectrometry: application to pharmacokinetic studies

A high-performance liquid chromatography (HPLC) method with tandem mass spectrometric detection is described for the determination of paroxetine, an antidepressant drug, and its metabolite (3S,4R)-4-(4-fluorophenyl)-3-(4-hydroxy-3-methoxyphenoxymethyl)piperidine (HM paroxetine) in human plasma. Plasma samples were hydrolysed with hydrochloric acid and then analytes were extracted with ethyl acetate at alkaline pH. Extracts were analysed by HPLC coupled to an atmospheric pressure ionisation-electrospray (ESI) interface and an ion trap mass spectrometer. Chromatography was performed on a reversed-phase column using acetonitrile/0.02% formic acid (66:34, v/v) as a mobile phase. The mass spectrometer was operated in the multiple reaction monitoring mode. The method was validated over concentration ranges of 0.75-100 microg/L and 5-100 microg/L for paroxetine and HM paroxetine, respectively. Mean recoveries of 77% for paroxetine and 76% for HM paroxetine were found, with precision always better than 15%. The limits of detection and quantification were 0.20 and 0.70 microg/L for paroxetine, and 0.70 and 2.20 microg/L for its metabolite. The method was applied to the analysis of plasma samples obtained from nine healthy male volunteers administered with a single oral dose of 20 mg paroxetine. After the 20-mg dose, the mean peak plasma concentration was 8.60 microg/L for paroxetine and 92.40 microg/L for HM paroxetine showing a tenfold ratio between the metabolite and the parent drug along the entire time-concentration curve.     

Liquid chromatographic/tandem mass spectrometric method for the quantitation of tranilast in human plasma

An analytical method for the determination of tranilast in human plasma using tramadol as the internal standard has been developed based on liquid chromatography/tandem mass spectrometry. Sample preparation involved protein precipitation with methanol. Separation by reversed-phase high-performance liquid chromatography using methanol/10 mM ammonium acetate (70: 30, v/v) as mobile phase was complete in a run time of 2.4 min. Detection on a Q TRAP system used multiple reaction monitoring. The method was linear in the range 0.06-20 microg/mL with intra- and inter-day precisions (as relative standard deviation) of 2.2-2.6% and 2.3-2.9%, respectively. Accuracy (as relative error) was <-2.5%. The method was applied in a pharmacokinetic study in healthy volunteers treated with a single 80 mg oral dose of tranilast.     

高效液相色谱法测定人血浆中的芦氟沙星

 建立了测定人血浆中芦氟沙星质量浓度的高效液相色谱法 ,血浆用二氯甲烷提取 3次 ,以 UltrasphereODS(4.6mm i.d.× 2 5 0 mm)为色谱柱 ,流动相为甲醇 -1 0 mmol/L 溴化四丁铵 -三乙胺 (体积比为 3 2∶ 68∶0 .5 ) ,用磷酸调 p H2 .8,检测波长 2 95 nm,流速为 1 .2 m L/min,以培氟沙星为内标。血浆中芦氟沙星的线性范围为 0 .1～ 1 0 mg/L ,最低检测质量浓度为 0 .0 5 mg/L ,回收率为 99.7% ,日内、日间 RSD分别为 2 .3 3 %和3 .83 %。方法简便、快速、准确 ,适用于人血浆中芦氟沙星质量浓度的测定。     

High-performance liquid chromatographic method with ultraviolet detection for the determination of dapsone and its hydroxylated metabolite in human plasma

A validated high-performance liquid chromatographic method with ultraviolet detection for the quantitative determination of dapsone (4,4'-diaminodifenyl sulfone, DDS) and a metabolite, hydroxylaminodapsone (4-amino-4-hydroxylaminodiphenyl sulfone, DDS-NOH), in human plasma is described. Human plasma was deproteinized with acetone and the clear supernatant solution after centrifugation was evaporated to dryness under a gentle stream of nitrogen at 70 degrees C. The residue was dissolved in a mixture of HPLC eluent and acetone (18:5 v/v) and an aliquot of this solution (50 microL) was injected onto the HPLC column. Dapsone, hydroxylaminodapsone and diazoxide as internal standard, were separated within 10 min by isocratic elution with water:acetonitrile:glacial acetic acid:triethylamine (80:20:1.0:0.5 by volume) as eluent. Detection was by ultraviolet at the wavelength of 295 nm. The within-day repeatability coefficients of variation were 3-5% for dapsone (0.301-20.0 mg/L, n = 5) and 3-5% for hydroxylaminodapsone (0.0948-6.32 mg/L, n = 5), whereas the between-day repeatability coefficients of variation were 3-8% (0.301-20.0 mg/L, n = 5) for dapsone and 4-10% for hydroxylaminodapsone (0.0948-6.32 mg/L, n = 5). The mean recoveries -were 92-107% (0.301-20.0 mg/L, n = 2), 80-82% (0.0948-6.32 mg/L, n = 2) and 88% (0.0200 mg/mL, n = 5), for dapsone, hydroxylaminodapsone and diazoxide, respectively. The average correlation coefficient of the calibration curve was 0.99988 (n = 5) for dapsone at a concentration range of 0.301-20.0 mg/L, whereas the average correlation coefficient of the hydroxylaminodapsone calibration curve was 0.99981 (n = 5) at a concentration range of 0.0948-6.32 mg/L. The limits of detection were 0.00200 and 0.0470 mg/L for dapsone and hydroxylaminodapsone, respectively. The method is suitable for drug level monitoring and for pharmacokinetic studies.     

Hydrophilic interaction chromatography-electrospray ionization tandem mass spectrometric analysis of anastrozole in human plasma and its application to a pharmacokinetic study

A hydrophilic interaction chromatography-electrospray ionization tandem mass spectrometric method was developed for determination of anastrozole in human plasma. Anastrozole and irbesartan (internal standard) were extracted from human plasma with a mixture of dichloromethane and methyl tert-butyl ether (30:70, v/v). Analysis of the analytes was performed on a Luna HILIC column with the mobile phase of acetonitrile-10 m m ammonium formate (95:5, v/v) and detected by electrospray ionization tandem mass spectrometry in the selected reaction monitoring mode. The standard curve was linear (r(2) = 0.9992) over the concentration range of 0.10-50.0 ng/mL using 200 μL of plasma sample. The coefficient of variation and relative error for intra- and inter-assay at four QC levels were 1.2-10.0% and -7.2-3.2%, respectively. The present method was applied successfully to the pharmacokinetic study of anastrozole after oral administration of 1 mg anastrozole tablet to healthy male volunteers.     

高效液相色谱法测定人血浆中的辛伐他汀

 建立了高效液相色谱法监测人口服辛伐他汀药物后的血药浓度。血样用环己烷-二氯甲烷(体积比为3.5∶1)提取,以洛伐他汀为内标,在237nm波长下检测;色谱柱:LichrospherC18(200mm×4.6mmi.d.,5μm),流动相:乙腈-水(体积比为70∶30);流速:1.2mL/min。血药浓度在0.25～50.0μg/L范围内与峰面积和内标峰面积的比值之间线性关系良好,日内及日间相对标准偏差(n=5)分别低于7.94%和8.58%,回收率高于93.3%。方法灵敏、准确、快速,适用于药物动力学和药效学研究。     

高效液相色谱法测定血清中头孢噻肟浓度

用固相萃取法处理样品,以扑热息痛为内标物、甲醇－醋酸钠／醋酸缓冲溶液作流动相,采用反相高效液相色谱法测定血清中头孢噻肟的浓度。头孢噻肟和内标物的平均回收率分别为９６．７％和９７．７％,头孢噻肟血清浓度在１０ｍｇ／Ｌ至１５０ｍｇ／Ｌ范围内有良好线性关系,最低检测浓度为２ｍｇ／Ｌ,日内和日间相对标准偏差分别在３．０％和４．１％以内。结果表明方法准确、简便。     

Rapid and sensitive HPLC-MS/MS method for pharmacokinetic assessment of ribavirin in healthy Chinese

A rapid and sensitive quantitative assay method was developed for determining ribavirin pharmacokinetic in human plasma. The chromatographic separation was achieved within 4.5 min using a SinoChrom ODS-BP column (4.6 x 150 mm, 5 microm) with acetonitrile-water (1 mmol/L ammonium acetate buffer, 0.1% formic acid; 15:85, v/v) at a constant flow rate of 0.8 mL/min. The MRM pairs were m/z 245.2 --> m/z 113.1 for ribavirin and m/z 226.1 --> m/z 152.1 for acyclovir (internal standard), respectively, with dwell times of 200 ms for each transition. The results showed calibration curve for ribavirin was linear over a concentration range of 1-1000 ng/mL. The lower limit of quantification (LLOQ) was 1 ng/mL ribavirin. Twenty healthy volunteers received a 300 mg oral dose of ribavirin. Blood samples were then collected up to 120 h postdosing. All plasma data were comodeled for ribavirin by using noncompartmental modeling. The single dose of ribavirin was well tolerated and no serious adverse effects occurred. The mean time to maximum concentration was about 1.25 h. The mean maximum concentration of drug in plasma for oral ribavirin was 250 ng/mL. The mean elimination half-life was 43.6 h. The present study describes a simple, specific, sensitive HPLC-MS/MS method for measuring plasma drug concentration and analyzing human pharmacokinetics of ribavirin.     

高效液相色谱法测定人血清中鬼臼乙叉甙浓度

建立了测定血清中鬼臼乙叉甙浓度的反相高效液相色谱方法。血清样品以乙酸乙酯提取,加表鬼臼毒噻吩糖甙作内标,以甲醇∶水（５５∶４５）为流动相,紫外２５４ｎｍ检测,最低检测浓度０．１ｍｇ／Ｌ,在药物浓度为０．５～５０ｍｇ／Ｌ范围内有良好的线性关系,Ｙ＝０．０１６０＋０．０３４０Ｘ,ｒ＝０．９９９１,回收率达９５．０％。日内、日间精密度分别为４．１６％和４．７６％（ｎ＝５）。用所建立的方法测定了患者的血清浓度,结果表明,方法简便、灵敏。     

高效液相色谱法测定吲哚美辛控释胶囊的血药浓度和生物利用度

采用ＯＤＳ柱,甲醇－稀磷酸溶液（７６２４）为流动相,２６０ｎｍ为检测波长,建立了测定血浆中吲哚美辛浓度的高效液相色谱法,并测定了吲哚美辛控释胶囊炎痛康的血药浓度。结果表明,血浆中吲哚美辛浓度在０．１２５～５．０ｍｇ／Ｌ范围内线性关系良好（ｒ＝０．９９９６）,检测限６２．５μｇ／Ｌ（Ｓ／Ｎ＝３１）,平均回收率为１００．４％,日内和日间ＲＳＤ均小于５％。１１位受试者单剂量口服炎痛康后的相对生物利用度为１０２．３８％。