反相HPLC法测定药用人参中多种人参皂甙的含量

采用HPLC法对不同产地药用人参中多种人参皂甙（GinsenosideRf、Re、Rd、Rb1、Rb2、Rg1、Rg2、Re）进行定量分析，流动相分别选用乙腈-0．05mol／L磷酸二氢钠（30∶70）和（20∶80），流速1ml／min，紫外检测波长203nm，色谱柱：YMCParkA-312ODS（6min×150mmid），柱温35℃，回收率均≥96.90％，RSD＜0.56％。该法操作简便，精密度高，重视性好，为评价药用人参的品质提供了参考依据。     

高效液相色谱法测定消痰咳片的含量

目的采用反相色谱法同时测定消痰咳片中两种主要成分甲氧苄啶和磺胺林的含量.方法以乙腈0.1%H3PO4(1585)为流动相,检测波长254nm,HPLC法测定含量.结果试验表明,甲氧苄啶和磺胺林在0.8～8ug范围内呈良好的线性关系,回归方程分别为Y=-1127.1+110.2x(r=0.9994),Y=-1852.3+256.2x(r=0.9996),相对标准偏差分别为2.1%和0.8%.结论该方法简便、准确、可靠.     

HPLC法测定佐米曲普坦的含量及有关物质

目的:建立HPLC法测定佐米曲普坦的含量及纯度.方法:采用Zorbax SB-C18色谱柱,分别以甲醇:0.025mol/L磷酸二氢钾(16:84)和甲醇:0.025 mol/L磷酸二氢钾:三乙胺(25:75:0.5,pH=3.5)为流动相,流速为1mL/min,在检测波长为220nm处检测.结果:本品在0.01mg/mL～0.15mg/mL浓度范围内呈直线关系,本品中杂质的最小检测限为0.01%.对4批样品进行检测均未检出杂质,而粗品检出明显杂质.结论:本方法可用于含量测定和有关物质的检查.     

Determination of matrine and oxymatrine in Sophora subprostata by CE

Shan-dou-gen is the dried roots of Sophora subprostata (Leguminosae) and a commonly used Chinese herbal drug in Taiwan. It possesses antipyretic, anti-inflammatory, analgesic effects and is used to treat sore throat and acute pharyngolaryngeal infections. To evaluate the quality of S. subprostata, a simple, rapid and accurate high-performance capillary electrophoresis (HPCE) method was developed for the assay of two alkaloids: matrine and oxymatrine. The electrolyte was a buffer solution containing 75% 130 mM phosphate buffer (NaH2PO4/H3PO4, pH 3.5) and 25% acetonitrile. Applied voltage was 10 kV and temperature was 30 degrees C. 2-(4-Hydroxyphenyl)ethylammonium chloride was used as an internal standard and detector set at 200 nm. The contents of matrine and oxymatrine of S. subprostata in several different samples of crude drugs and commercial concentrated preparation have also been determined.     

Liquid chromatographic determination of fexofenadine in human plasma with fluorescence detection

A simple and sensitive method was developed for determination of fexofenadine by liquid chromatography with fluorescence detection. Fexofenadine in human plasma was extracted on a C18 bonded-phase extraction cartridge. The mobile phases were: (A) 0.05 M KH2PO4 buffer/acetonitrile/methanol (60:35:10, v/v/v) and (B) 0.05 M KH2PO4 buffer/acetonitrile (40:60, v/v). Chromatographic separation was achieved on an ODS-80A column (150 mm x 4.6 mm i.d., particle size 5 microm) using a linear gradient from A to B in 10 min. The peak was detected using a fluorescence detector set at Ex 220 nm and Em 290 nm, and the total time for a chromatographic separation was approximately 17 min. The validated quantitation ranges of this method were 1.0-500 ng/ml with coefficients of variation of 0.6-9.1%. Mean recoveries were 72.8-76.7% with coefficients of variation of 2.7-5.8%. This method is successfully applicable for therapeutic drug monitoring in patients treated with clinical doses of fexofenadine and for analyses within pharmacokinetic studies.     

Vasoactivity of trimetazidine on guinea-pig isolated ductus arteriosus.

The effect of trimetazidine (TMZ), an anti-anginal drug, on the mechanical response of the guinea-pig ductus arteriosus placed under conditions of mild hypoxia (PO2 approximately equal to 75 mmHg) was investigated. When the PO2 of the bathing solution was 75 mmHg, TMZ caused a dose-dependent increase in tension. The median effective dose (ED50) for the drug was 8 X 10(-5)M. TMZ-induced increase in tension was not significantly affected by pretreatment of the preparation with adrenoceptor blocking agents, or indomethacin. The amplitude of the PO2-dependent tension was significantly augmented by exposure of the strip to TMZ 10(-4)M, whereas neither the resting tone (low PO2), nor the oxygen-induced contraction (high PO2) were altered. This ability of TMZ to increase the tension response during hypoxia was dependent on the external calcium concentration. Under low PO2 conditions, a contractile activity of 10(-4)M TMZ was unmasked in preparations perfused with 18 mM K+-PSS medium. This response to TMZ disappeared after the removal of calcium from the bath. At the maximally effective dose of 10(-3)M, and during low PO2, the TMZ-induced contractile response changed to a relaxation response when the external K+ concentration was raised more than five fold. The possibility that TMZ stimulates the mechanism by which oxygen normally controls the concentration of free intracellular calcium in the ductus arteriosus is proposed.     

Determination of anticonvulsive preparations in the blood serum of patients by high-performance liquid chromatography

A method for simultaneous measurement of hexamydine, phenobarbital, diphenin and carbamazepine concentrations in serum using high performance liquid chromatography is described. The procedure employs acetonitrile extraction of anticonvulsants and chromatography of the extract under the following conditions: a column containing lichrosorb RP-8 10 microns (250 x 4 mm), mobile phase consisting of 30 vol.% ethanol solution in 0.01 M KH2PO4 pH 5.3, flow rate 0.5 ml/min, column temperature 30 degrees C, injection volume 20 microliters, detector wavelength 220 nm. Hexenal is used as an internal standard. The concentration range is 5-50 mg/l for phenobarbital, diphenin and carbamazepine and 5-30 mg/l for hexamydine. The relative standard deviation varies between 0.018 and 0.057 for therapeutic and toxic concentrations.     

HPLC-荧光检测法测定人血浆中厄贝沙坦的浓度

目的:建立以HPLC-荧光检测法测定人血浆中厄贝沙坦浓度的方法。方法:色谱柱为Diamonsil C18,流动相为0.02mol方芸L-1磷酸二氢钾-乙腈(50∶50),荧光激发波长为250nm,发射波长为375nm,流速为1.0mL·min-1,柱温为40℃。结果:厄贝沙坦检测浓度在1.0~1000ng·mL-1范围内线性关系良好(r=0.9998);低、中、高3种浓度(2.0、50.0、500.00ng·mL-1)的平均相对回收率分别为97.4%、106.1%、101.6%,日内、日间RSD均小于10%。结论:本方法简便、快速、准确、特异性和灵敏度高,可用于厄贝沙坦的血药浓度测定和药动学研究。     

高效液相色谱法测定小鼠纹状体中多巴胺的含量

目的:建立测定小鼠纹状体中多巴胺含量的紫外检测-高效液相色谱方法。方法:将小鼠处死,取大脑中的纹状体,用高氯酸除蛋白,采用高效液相色谱法在280 nm处测定,流动相为0.05 mol.L-1磷酸二氢钠-0.02 moL.L-1柠檬酸-甲醇(74∶24:∶2),流速为1.0mL.min-1,外标法定量。结果:色谱图显示多巴胺成分分离良好。多巴胺在0.78～15.50 mg.L-1范围内药物浓度与峰面积线性关系良好,r=0.999 0,相对回收率在85%～115%的范围内,RSD在2.6%～15.2%之间。结论:本法测定操作简便,灵敏度良好,结果准确可靠,可用于检测小鼠脑组织纹状体中多巴胺的含量。     

Determination of the anticancer drug, 15-deoxyspergualin, in plasma ultrafiltrate by liquid chromatography and precolumn derivatization with naphthalene-2,3-dicarboxaldehyde/cyanide

An alternative analytical method for the determination of 15-deoxyspergualin in plasma is described. The drug was initially separated from the plasma matrix by ultrafiltration and a precolumn derivatization step was performed with naphthalene-2,3-dicarboxaldehyde in the presence of sodium cyanide to yield the fluorescent N-substituted 1-cyanobenz[f]isoindole (CBI) derivative. The CBI derivative was separated and quantitated by reversed-phase chromatography using an ODS Hypersil column and mobile phase of KH2PO4 (0.1 M)-H3PO4-acetonitrile (48:0.8:52, v/v/v) containing dodecyl sodium sulphate (18 mM). The excitation and emission wavelengths for the fluorescence detector were 420 and 490 nm, respectively. The peak height was linearly related to drug concentration over the range from 5 ng ml-1 (10 nM) to 10 micrograms ml-1 (20 microM) in phosphate buffer (0.1 M, pH 7.0), spiked plasma ultrafiltrate and ultrafiltrate obtained from spiked plasma. Measurements could be made with a relative standard deviation of 4.5% or less in phosphate buffer (0.1 M, pH 7.0), 6.1% or less in spiked plasma ultrafiltrate and 12% or less in ultrafiltrate obtained from spiked plasma.     

一叶萩碱的高效毛细管电泳手性分离及其大鼠体内立体选择性代谢研究

目的建立一叶萩碱(SE)的高效毛细管电泳手性分离方法。方法以羟丙基-β-环糊精(HP-β-CD)为手性选择剂,测定条件为:分离介质32 mmol·L^-1 HP-β-CD的Tris-H₃PO₄缓冲液(40 mmol·L^-1,H₃PO₄调至pH 6.0);分离电压15 kV,柱温16℃,压力进样6 s,检测波长254 nm;大鼠各生物样品碱化后乙酸乙酯萃取。结果测定条件下SE基本达到基线分离,大鼠生物样品测定不受内源及代谢物干扰。大鼠ip SE经胆汁、尿和粪排泄以D型为主,具有立体选择性。结论本法简便可靠,可适用于SE在大鼠体内立体选择性代谢研究。     

高效液相色谱法测定人血浆中缬沙坦的药物浓度

目的 :测定人血浆中缬沙坦的药物浓度。方法 :采用液固萃取法提取 ,高效液相色谱法测定。色谱柱 :HypersilODSC18(4 6nm×200nm ,5μm ) ;流动相 :乙腈 -0 01mol/L的磷酸盐缓冲液 (50∶50 ,pH2 8) ;流速 :1 5ml/min ;荧光检测器 :λex为265nm ,λem为378nm。结果 :缬沙坦的保留时间为5 4min ,定量线性范围0 05～5μg/ml,方法回收率>90 % (n=5) ,日内、日间RSD<10 % (n=5)。结论 :本法快速 ,定量准确 ,可用于血药浓度测定及人体药代动力学研究     

HPLC法测定镇痛复方制剂阿司匹林萘磺酸右丙氧芬片含量及对其分解产物的定量检查

本文介绍了用高效液相色谱法测定阿司匹林、萘磺酸右丙氧芬片含量及其分解产物水杨酸含量的方法。采用 μ-BondapakC18 为固定相 ,0.02mol·L-1 磷酸二氢钾 -甲醇 -四氢呋喃(THF)(2:1:0.1)为流动相 ,紫外检测器于230nm波长处测定 ,方法准确可靠 ,对阿司匹林和萘磺酸右丙氧芬的回收率分别为99.25 %(RSD0.78 %)、99.7 %(RSD1.05 %)。由于阿司匹林不稳定 ,易分解成水杨酸 ,影响制剂质量。本方法的色谱条件可使阿司匹林、水杨酸、萘磺酸右丙氧芬完全分离 ,因此可同时用于水杨酸含量的检查。     

HPLC法测定蒙药肝乐康胶囊中氧化苦参碱含量

目的:建立蒙药肝乐康胶囊的质量标准。方法:用高效液相色谱法对处方中苦参有效成分氧化苦参碱进行定量分析。采用lnertsilNH2Columns(250mm×4.6mm,5um)色谱柱,流动相:乙腈:3%磷酸水:无水乙醇(80∶10∶10),流速0.1ml/min,柱温30℃,检测波长:220nm。结果:氧化苦参碱进样量在75～375μg范围内与峰面积线性关系良好(r=0.9997)。平均加样回收率为103.2%(RSD=1.12%,n=5)。结论:本试验方法既先进又简便,结果准确可靠,为该制剂的质量标准提供可靠依据。     

高效液相色谱法测定消痰咳片的含量

目的：采用反相色谱法同时测定消痰咳片中两种主要成分甲氧苄啶和磺胺体的含量。方法：以乙腈：0.1%H3PO4(15:85)为流动相，检测波长254nm，HPLC法测定含量。结果：试验表明，甲氧苄啶和磺胺林在0.8-8ug范围内呈良好的线性关系，回归方程分别为Y＝－1127.1＋110.2x(r=0.9994),Y=-1852.3 256.2x(r=0.9996),相对标准偏差分别为2.1%和0.8%。结论：该方法简便、准确、可靠。     

HPLC测定泛酸钙的有关物质

目的建立高效液相色谱法测定泛酸钙的有关物质。方法用十八烷基硅烷键合硅胶为填充剂;以磷酸盐缓冲液(取磷酸二氢钾8.34 g与磷酸氢二钾0.87 g,加水1 000 mL溶解,用磷酸调节pH值至5.7)为流动相;检测波长为205 nm。结果杂质峰与主峰能够得到有效的分离,特殊杂质泛解酸的最低检出限为1.33 ng,最低定量限为4.42 ng;3批泛酸钙样品经检测泛解酸含量分别为0.234%,0.222%,0.234%,其他总杂质分别为0.168%,0.165%,0.157%。结论该方法准确可靠,能有效检测出泛酸钙中的有关物质。     

反相高效液相色谱法测定大鼠血浆中水飞蓟宾的浓度

测定三组Wistar大鼠分别灌胃给与受试制剂和两组参比制剂后不同时刻血浆中水飞蓟宾的浓度。采用色谱柱为KromasilC18柱 (5 μm粒径 ,2 0 0mm× 4 6mmI .D .) ,流动相为乙腈 甲醇 磷酸二氢胺缓冲液 (体积比为 2 4∶2 4∶5 0 ,pH =5 ) ,检测波长为UV 2 88nm。 0 2 5～ 2 0 0 0mg/L范围内线性关系良好 (r =0 9976 ) ,日内 ,日间RSD分别≤ 5 99%和≤ 6 91%。方法简便快速 ,适用于该药的动物生物利用度试验研究     

反相离子对色谱法测定附子中生物碱成分

目的测定附子中乌头碱、新乌头碱、次乌头碱、北乌碱、苯甲酰乌头原碱和苯甲酰新乌头原碱等6种生物碱的含量。方法用反相离子对HPLC法，使用AichromBond-1 C₁₈柱(250 mm×4.6 mm ID)；流动相：乙腈-5 mmol·L^-1 NaH₂PO₄溶液，磷酸调至pH 4.5(50∶50)，内含7 mmol·L^-1 十二烷基硫酸钠(SDS)；检测波长：235 nm；流速：1.0 mL·min^-1；柱温：35 ℃。结果以上6种生物碱可以完全分离，准确测定。结论该方法准确度高，可应用于附子中生物碱的含量测定。