HPLC法测定人血浆中奥美拉唑的浓度

目的：了解人血浆中奥美拉唑浓度。方法：使用内标法,对10名健康志愿者的奥美拉唑血药浓度进行HPLC法检测。结果：分析结果显示,HPLC法的方法回收率为98.32%-104.96%,线性范围10~2000μg/L;10名志愿者的tmax=（2.09±0.75）h,t1/2=（1.02±0.58）h,ρmax=（774.56±340.46）μg/L,MRT0→1=（3.02±0.83）h,AUC0→12=（1751.42±1230.68）μg·h/L,AUC0→∞=（1784.50±1298.44）μg·h/L。结论：HPLC法测定奥美拉唑浓度,其灵敏度高,专属性强,准确,简便。     

HPLC法测定狗血浆中奥美拉唑的含量

目的建立奥美拉唑狗血药浓度高效液相色谱测定方法.方法色谱柱为Hypersil C18(200mm×4.0mm,5μm),流动相为甲醇-水(65∶35),流速为0.8mL·min-1,紫外检测器波长为302nm,乙奈酚为内标,血样用正己烷提取,进样量50μL,柱温:30℃,峰面积比定量.结果标准曲线线性范围25~500ng·mL-1,r=0.9984,血样加内标绝对提取回收率80.3%~94.0%,相对回收率95.0%~95.7%,最低检测限25ng·mL-1.结论本方法简便、快速、准确、重现性好,可适用于奥美拉唑药代动力学研究.     

高效液相色谱法测定奥美拉唑肠溶胶囊中奥美拉唑的含量

目的 建立奥美拉唑含量的高效液相测定方法.方法 采用C8(5μm,4.6mm×250mm)色谱柱,流动相为磷酸盐缓冲液-乙腈(70∶30),检测波长为280nm.结果 奥美拉唑在49.48μg·mL-1～395.84μg·mL-1范围内线性良好,相关系数r=0.99998;平均回收率为99.8%(n=9,RSD为0.8%).结论 本方法重现性良好,回收率较高,可作为奥美拉唑肠溶胶素的质量控制标准.     

高效液相色谱法测定奥美拉唑肠溶胶囊中的奥美拉唑磺酰化物

目的建立奥美拉唑肠溶胶囊中奥美拉唑磺酰化物的测定方法。方法色谱柱:Zorbax C8(4.6 mm×250 mm);流动相:0.01mol.L-1磷酸氢二钠-乙腈(75∶25);流速1.0mL.min-1;检测波长302nm;进样量20μL。结果奥美拉唑磺酰化物在0.6μg.mL-1~1.4μg.mL-1范围内呈良好的线性关系(r=0.9998,n=5)。平均回收率102.2%,RSD=1.27%。结论本方法简便,迅速,准确。     

反相高效液相色谱法测定人血浆中甲氨蝶呤的浓度

目的:建立反相高效液相色谱法测定人血浆中甲氨蝶呤浓度的方法. 方法:使用岛津LC-10AD高效液相色谱仪,Lichrosphere C18柱(5 μm,4.6 mm×250 mm),流动相为 0.025 mol·L-1 NaH2PO4溶液(pH5.5)-甲醇(72∶28),检测波长 313 nm,流速 1.0 mL·min-1, 柱温35℃,内标为阿魏酸.结果:甲氨蝶呤浓度在0.05～5.00 μg·mL-1范围内线性关系良好,回归方程为Y=3.094 2c 0.006 8(r=0.999 3),日内变异系数小于7%,日间变异系数小于10%;检测限为 20 ng·mL-1.结论:本法操作简便,适用于甲氨蝶呤的血药浓度测定及药代动力学研究.     

简单灵敏的HPLC法测定人血浆中头孢丙烯浓度

目的:建立血浆中头孢丙烯的HPLC检测方法.方法:采用高效液相色谱检测法,分析柱为Hypersil BDS C18 (200 mm×4.6 mm,5μm),流动相为20 mmol/L乙酸铵/10％乙酸(pH=3.7):乙腈=92:8(V/V),流速1.0 mL/min,柱温30℃,检测波长282 nm,进样量20μL.血浆样品用三氟醋酸直接沉淀后,取上清进样分析.结果:头孢丙烯在0.10～10.01 μg/mL范围内线性关系良好(r=1.0000),最低定量浓度为0.10μg/mL,日内日间RSD均＜15％(n=15).结论:研究建立的HPLC法快速、简便、高效,精密度和准确度高,适合血样中头孢丙烯浓度的检测.     

高效液相色谱法快速测定黄体酮血药浓度

目的建立高效液相色谱法快速测定人血浆中黄体酮血药浓度。方法色谱柱为Hypersil ODS2（5μm,4.6mm×250mm）;流动相为乙腈：5mmol/L三羟甲基氨基甲烷（pH=8.0）=63：37;柱温：室温;流速1.0ml/min;检测波长：240nm。结果本测定方法的线性范围：10～1600ng/ml,r=0.9998。平均回收率为（96.1±3.1）%,日内RSD≤5.7%,日间RSD≤6.4%。黄体酮的最低检测浓度为6ng/ml。结论本方法简单、快速、灵敏、重现性好,适用于黄体酮临床血药浓度监测及人体药代动力学研究。     

奥美拉唑在健康人体内的药物动力学研究

本实验建立了奥美拉唑在人体内血药浓度的ＨＰＬＣ测定方法，并对奥美拉唑片（供试品）及胶囊剂（对照品）在健康人体内的药物动力学进行了研究。结果表明，奥美拉唑片与胶囊剂的达峰时间（Ｔｍ）分别为３．３ｈ和３．５ｈ（Ｐ＞０．０５）；Ｃｍ分别为７７４．５ｎｇ／ｍｌ和６１６．５ｎｇ／ｍｌ（Ｐ＜０．０５）；ＡＵＣ分别为３２７４．９（ｎｇ·ｈ）／ｍｌ和２９６８．１（ｎｇ·ｈ）／ｍｌ（Ｐ＜０．０５）。供试品的相对生物利用度为１０７．０±０．０９％，显示奥美拉唑片生物利用度优于对照品。但以２０％作为等效性判断检验标准，两者显示生物等效。     

高效液相色谱法测定人血中氢溴酸右美沙芬浓度

目的研究氢溴酸右美沙芬在健康志愿者体内的血药浓度。方法采用高效液相色谱法测定8例健康受试者口服右美沙芬糖浆和片剂后不同时间血浆中的美沙芬浓度。结果右美沙芬在5--500 ng/ml浓度范围内呈良好线性关系（r=0.9965）。结论本法精密,准确,可用于氢溴酸右美沙芬的药动学研究。     

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法测定人血浆中咖啡因含量的不确定度评定

目的对高效液相色谱法测定血浆中咖啡因的不确定度进行分析,找出影响因素,对不确定度进行评估,如实反映测量的置信度和准确度。方法采用ACE 5 C18-AR柱(150 mm×4.6 mm,5μm),流动相:甲醇-0.2%醋酸溶液(17∶83),检测波长:273 nm,流速:1.0 mL/min,测定咖啡因含量后,建立数学模型,分析过程中各分量引起的不确定度,采用A类评定程序评价随机效应引起的不确定度,B类评定程序评价其他因素引起的不确定度。结果置信概率P为95%时,血浆中咖啡因可表示为:低浓度(1 058.08±29.24)ng/mL,中浓度(3 489.53±90.21)ng/mL,高浓度(8 453.32±115.92)ng/mL。结论该方法适用于HPLC法测定血浆中咖啡因浓度的不确定度评定,能为复杂生物样品分析过程的不确定度评定提供一定参考。     

HPLC同时测定血浆中头孢氨苄和甲氧苄啶的浓度

采用高效液相色谱紫外检测器同时检测血浆中头孢氨苄和甲氧苄啶的浓度。以0.5倍血浆体积,浓度为10%(v/v)的高氯酸为蛋白沉淀剂。色谱条件:Diamonsil C18(250mm×4.6mm,5μm),柱温:30℃,流动相:pH3.0的0.05mol/L的磷酸盐缓冲液∶乙腈∶甲醇(76∶16∶8),流速1.0ml/min,进样量20μl,检测波长240nm。头孢氨苄、甲氧苄啶及内源性物质分离良好。头孢氨苄血药浓度线性范围为0.5~50.0μg/ml,检测限为50ng/ml,高、中、低浓度的相对回收率在97.3%~100.5%之间(n=5),日内RSD≤6.5%(n=5),日间RSD≤8.3%(n=5)。甲氧苄啶血药浓度线性范围为0.25~25.0μg/ml,检测限为25ng/ml,高、中、低浓度的相对回收率在96.5%~99.3%之间(n=5),日内RSD≤6.9%(n=5),日间RSD≤8.6%(n=5)。本法样品处理简单、灵敏、准确,适合于同时测定两者的体内浓度。     

HPLC法测定人血浆中奥美拉唑浓度

目的建立人血浆中奥美拉唑的HPLC测定方法,并对奥美拉唑在健康志愿者体内进行药动学研究。方法采用内标法,以乙醚进行提取,提取液吹干,残渣用甲醇溶解后进行HPLC法检测;色谱柱为DiamonsilC18(150mm×4.6mm,5μm),流动相为甲醇-乙酸胺缓冲液(58∶42,V/V),其中缓冲液组成为水-醋酸-三乙胺(98∶1∶1,V/V),流速1.0mL·min-1,检测波长302nm。测定了24名健康志愿者单剂量口服40mg奥美拉唑胶囊后不同时刻奥美拉唑血药浓度,并采用DAS软件对其体内药动学参数进行估算。结果本测定方法的方法回收率为98.34%~105.87%,线性范围为10~2000μg·L-1。24名健康志愿者体内药动学采用统计矩分析,tmax为(2.11±0.73)h,t1/2为(1.03±0.56)h,ρmax为(776.30±341.55)μg·L-1,MRT0→t为(3.04±0.80)h,AUC0→12为(1749.90±1241.73)μg·h·L-1,AUC0→∞为(1790.48±1309.45)μg·h·L-1。结论本方法灵敏度高,重现性好,专属性强,适合临床药动学研究。     

A simple HPLC method for doxorubicin in plasma and tissues of nude mice

Doxorubicin is a cytotoxic anthracycline that has been used for the treatment of several malignancies. Several HPLC methods have been reported for the quantification of doxorubicin in biological samples. Tissue matrix effect and sample size requirements, however, have been remaining issues for simple and easy-to-adapt analytical methods in small animal experiments. The present study established a simple HPLC method for doxorubicin in plasma and tissues (tumor, heart, spleen, liver, gastrointestinal tract, brain, lung, and kidney) of nude mice. Our method required a small sample volume (100 μL plasma and 10 mg tissue), which made it possible to use each blank tissue for calibration curves. The limit of quantification was 25 ng/mL in plasma and 0.1 to 0.4 μg/mg in other tissues with recovery rates ranging from 52.4 to 95.2%. The linearity, accuracy and precision in all tissues, except gastrointestinal tract (GIT), were found to be acceptable in the range of 25–2000 ng/mL plasma and 0.1–4 ng/mg tissue. This method was used successfully to determine the drug concentration in plasma and tissues of human tumor xenograft-bearing nude mice given intratumoral doxorubicin in a polymeric drug delivery system designed for sustained release. In conclusion, the present method may be useful as a simple and easy-to-adapt, yet, sensitive analytical method of doxorubicin for plasma and tissue pharmacokinetic studies in small animals such as nude mice.     

An HPLC method for the simultaneous determination of neurotoxic dipyridyl isomers in human plasma

Several studies on dipyridyl isomers have suggested that they are neurotoxic and that chronic exposure to these compounds could be a potential human health hazard. A reversed phase HPLC method was developed for the simultaneous quantitation of 2,2'-dipyridyl and its four positional isomers, 2,3'-, 2,4'-, 3,4'- and 4,4'-dipyridyl in human plasma. Plasma samples were basified, extracted with 1-chlorobutane, evaporated, the residue reconstituted in mobile phase, and an aliquot part was analyzed by HPLC. Chromatographic separations were performed on a C(18) reversed phase Sunfire column eluted with a mobile phase composed of potassium phosphate (pH 3.5; 25 mM)-acetonitrile (80:20, v/v). Isomers were separated with good resolution, and quantification was determined utilizing an internal standard of quinoxaline. The method has been validated over a range from 30 to 2000 ng/ml with correlation coefficients higher than 0.995. Extraction recoveries for the dipyridyl isomers averaged from 65 to 92%. Limit of detection and limit of quantitation for the dipyridyl isomers ranged from 15 to 70 ng/ml and 30 to 90 ng/ml, respectively. The inter- and intra-day variation did not exceed 7% with an accuracy range of 96-102%. The described analytical method was successfully utilized for the determination of dipyridyl isomers in human plasma and suggested the need for more routine monitoring of tobacco smokers and other individuals who are involuntarily exposed to environmental source of dipyridyl isomers.     

HPLC法测定血浆中奥美拉唑及其人体药动学研究

目的建立测定血浆中奥美拉唑的HPLC法 ,并对其进行药代动力学研究。方法以CapcellPak C18柱 ,(4 6mm× 15 0mm ,5 μm,SHISEIDOFINECHEMICALS ,日本 )为色谱柱 ,以乙腈 0 0 5mol·L-1磷酸二氢铵 (V∶V =35∶6 5 )为流动相 ,测定了 18名健康男性志愿受试者单剂量口服奥美拉唑胶囊后的不同时刻血浆中奥美拉唑的质量浓度 ,并根据测定结果求算奥美拉唑的药代动力学参数。结果 18名健康受试者口服奥美拉唑胶囊后 ,血浆中的tmax为 (2 3± 0 8)h ;ρmax为(10 5 0 0± 396 0 ) μg·L-1;t1/ 2 为 (1 3± 0 5 )h ;AUC0 -10 为 (32 4 8 9± 2 15 2 1) μg·h·L-1;AUC0 -∞ 为 (3393 9± 2 342 6 ) μg·h·L-1。结论该方法适合临床药代动力学研究     

高效液相色谱法测定去甲万古霉素血药浓度

目的：建立人血浆中去甲万古霉素反相高效液相色谱测定法,为临床监测血药浓度提供方法学基础。方法：采用液－液萃取法并选用２万古霉素为内标,以ＹＷＧ－ＲＰ１８色谱柱,流动相为乙腈－０．０５ｍｏｌ．Ｌ＾－１磷酸二氯（８：９２）,紫外２３６ｎｍ检测。结果：本法在０．８１～８１ｕｇ．ｍｌ＾－１间线性良好,相关系数ｒ＝０．９９９８（ｎ＝６）。日内日间精密度ＲＳＤ均小于３％,提取回收率均大于７５％。结论：本方法在     

Effect of omeprazole and cimetidine on plasma diazepam levels

Summary The effects of steady state dosing with omeprazole and cimetidine on plasma diazepam levels have been studied in 12 healthy males. Single doses of diazepam (0.1 mg · kg⁻¹ i.v.) were administered after one week of treatment with omeprazole 20 mg once daily, cimetidine 400 mg b. d. or placebo, and the treatment was continued for a further 5 days. Blood was collected for 120 h after the dose of diazepam for the measurement of diazepam and its major metabolite desmethyl diazepam. The mean clearance of diazepam was decreased by 27% and 38% and its half-life was increased by 36% and 39% after omeprazole and cimetidine, respectively. Neither drug had any apparent effect on the volume of distribution of diazepam. Desmethyldiazepam appeared more slowly after both omeprazole and cimetidine. It is concluded that the decrease in diazepam clearance was associated with inhibition of hepatic metabolism both by omeprazole and cimetidine. However, since diazepam has a wide therapeutic range, it is unlikely that concomitant treatment with therapeutically recommended doses of either omeprazole or cimetidine will result in a clinically significant interaction with diazepam.     

HPLC测定血浆中头孢拉定的浓度

目的建立测定血浆中头孢拉定浓度的方法。方法采用HPLC法。用Eclipse XDB-C8色谱柱(150 mm×4.6 mm,5μm),以乙腈-磷酸盐缓冲液(17∶83)为流动相,N-对甲氧基苯甲酰基丁酸(ABA)为内标,于254 nm测定。结果头孢拉定在0.5~30.0μg.ml-1浓度范围内线性良好,最低定量浓度为0.5μg.ml-1,日内RSD<8%,日间RSD<13%,平均相对回收率99.1%。结论所建方法操作简单、快速、重复性好、准确可靠,可用于临床血药浓度的监测及药动学的研究。     

高效液相色谱法测定人血清中地西泮血药浓度及临床监测

目的 建立人血清中地西泮浓度测定的高效液相色谱法(HPLC),并用该法测定临床病人静脉滴注地西泮后的血药浓度.方法 人血清样品采用正戊烷萃取进行分析.色谱柱:SB-C18色谱柱(150 mm×4.6 mm,5 μm),流动相为甲醇-水-四甲基乙二胺-冰醋酸(670:330:2.2:1.76),柱温:40 ℃,流速:0.8 mL·min-1,检测波长:254 nm,进样量:20 μL.以氯氮平作为内标物.结果 地西泮在10~1 200 μg·L-1浓度范围内,峰面积与其浓度呈良好的线性关系(r=0.998 47),定量下限为10 μg·L-1.地西泮的高、中、低3种浓度相对平均回收率>95%,提取回收率均>70%,日内、日间的RSD均<15%(n=5).地西泮稳定性考察RSD均<15%(n=5).地西泮线性方程:Y=2 205.2X+1 876.1(r=0.998 47).临床20例病人分别滴注地西泮20 mg,1 d 2次,前5 d早晨治疗前采血均检测出地西泮血药浓度.结论 该方法灵敏度高,操作简便、快速、准确,可用于人血清中地西泮血药浓度监测,并为临床病人个体化给药提供参考.