人血清中地尔硫高效液相色谱法测定及药代动力学参数

建立了反相高效液相色谱法监测人口服地尔硫艹卓缓释片后血药浓度。血样用正己烷－氯仿－异丙醇混合溶剂（６０４０５）提取后，以Ｃ１８化学键合硅胶为固定相，甲醇－水－三乙胺为流动相，安定为内标，在２３９ｎｍ波长处定量检测。血药浓度在１５～３００μｇ／Ｌ范围内线性关系良好，最低检测浓度为３μｇ／Ｌ。批内（ｎ＝７）及批间（ｎ＝５）测定相对标准偏差分别小于６．８％和８．４％，回收率为９１％～１０４％。监测了８名健康人口服盐酸地尔硫艹卓缓释片后的不同时间的血药浓度变化，计算了有关的药代动力学参数。     

用钨酸盐和耐尔蓝光度法测定痕量碲

报告一个简单、灵敏、快速光度测定碲的方法。聚乙烯醇（ＰＶＡ）存在下，碲与钨酸盐和耐尔蓝（ＮＢ）反应形成离子缔合物。离子缔合物的最大吸收峰位于５８０ｎｍ；表观摩尔吸光系数ε值为３．３３×１０＾７Ｌ·ｍｏｌ＾－１·ｃｍ＾－１。本方法允许的碲浓度范围为０￣６．０μｇ／Ｌ；对４．８μｇ／Ｌ碲（Ⅳ）测定的相对标准偏差为１．３％（ｎ＝１１）；检测限（３σ）为０．０１１μｇ／Ｌ（ｎ＝１２）。考察了许多离子的影响     

气相色谱/质谱法测定大鼠脑中5-羟色胺的含量

采用气相色谱／质谱法（ＧＣ／ＭＳ）测定了正常大鼠和服药大鼠脑组织中５－羟色胺（５－ＨＴ）的浓度。大鼠脑组织制成匀浆后,先将５－ＨＴ酰化,酰化物经乙酸乙酯提取后,再经七氟丁酸酐衍生化,用ＧＣ／ＭＳ测定。ＭＳ采用电子捕获负离子化学电离（ＥＣＮＩＣＩ）模式。方法的线性范围为０．５０～５０．０μｇ／Ｌ,回归方程为Ｙ＝０．１３４８Ｘ－０．０７９９５（ｒ＝０．９９９６）;平均回收率为９８．２％±３．８％（ｎ＝１０）;检测限为０．５μｇ／Ｌ;相对标准偏差小于１０％。     

铜钨杂多酸—耐尔蓝离子缔合显色反应及其应用

在阿拉伯胶存在下铜钨多酸与耐尔蓝形成离子缔子缔合物，其最大吸收位于５８０ｎｍ；表观摩尔吸光度ε值为２．２２＊１０＾６Ｌ．ｃｍ ＾－１；铜量在０－２４μｇ／Ｌ范围内服从比耳定律；检测限（３σ）１．０μｇ／Ｌ（ｎ＝１０）；分析１６μｇ／Ｌ铜的ＲＳＤ＝１．５％（ｎ＝１１）；离子缔合物的摩尔比为Ｃｕ：Ｗ：ＮＢ＝１：１２：４。     

高效液相色谱法测定全血环孢霉素A的浓度

建立了高效液相色谱法测定全血环孢霉素Ａ 浓度的方法。全血样品经多步处理后以２０ μＬ注入ｒｅｏｓｏｌｖｅ Ｃ１８,５μ色谱柱,采用Ｖ（乙腈）∶Ｖ（水）＝ ８０∶２０ 的流动相,在７５℃柱温下,以１ ｍ Ｌ／ｍ ｉｎ 流速洗脱,检测波长为２０８ｎｍ 。环孢霉素Ａ 的回收率为９９％ ～１０４ ％ ,相对标准偏差＜ ３．４２％ （ｎ＝ ５） ,日间＜ ８．１９％ （ｎ＝ ４） 。最低检测浓度为２５ μｇ／Ｌ。     

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％。     

用金钨杂多酸和耐尔蓝光度法测定纳克量金

在阿拉伯胶存在下，金与钨酸钠和耐尔蓝（ＮＢ）形成离子缔合物，它的最大吸收位于５８０ｎｍ，表观摩尔吸光系数ε值为２．３８×１０＾７Ｌ·ｍｏｌ＾－１·ｃｍ＾－１，体系至少稳定２４ｈ。金量在０￣４．４μｇ／Ｌ范围内服从比尔定律，检测限（３σ）为０．０６９μｇ／Ｌ（ｎ＝１２），对４．０μｇ／Ｌ Ａｕ（Ⅲ）测定的相对标准偏差为１．９％（ｎ＝１１），离子缔合物的摩尔比为Ａｕ（Ⅲ）：ＮＢ＝１：３。考察了４０多种     

高效液相色谱法快速测定人血清中丙戊酸含量

建立了血清中丙戊酸的高效液相色谱快速分析法。用ＺｏｒｂａｘＯＤＳ柱,ｐＨ４．２硫酸水溶液为流动相,检测波长２１０ｎｍ,流速０．８ｍＬ／ｍｉｎ,线性范围０．８２μｍｏｌ／Ｌ～１．８ｍｍｏｌ／Ｌ（ｒ＝０．９９６）,最低检测限０．８２μｍｏｌ／Ｌ,平均回收率为９８．３２％±２．２７％,日内与日间的变异系数分别为３．３１％（ｎ＝５）和４．８２％（ｎ＝７）。     

甲硝唑的伏安研究及其分析应用

本研究了甲硝唑在金微上电极上的３伏安行为，考虑了底液、人体内微量共存物质及表面活性剂对甲硝唑还原行为的；知０．２ｍｏｌ／Ｌ柠檬酸二氧钾底液中，甲硝唑的浓度与ｉｐ（Ｅｐ＝－０．４６ＶＵＳ Ａｇ／ＡｇＣｌ）在０．５０－２２００μｇ／ｍＬ范围内存在良好的线性关系，在检测限为０．２０μｇ／ｍＬＲＳＤ为５．０４％（ｎ＝８）．电极过程为一含有咐附的受扩散控制的不可逆氧化还原过程。     

丁基罗丹明B—钼酸盐光度法连续测定铈和钪

在聚乙烯醇（ＰＶＡ）存在下，丁基罗丹明Ｂ（ＢＲＢ）分别与铈钼、钪钼杂多酸络阴离子形成离子缔合物，其最大吸收均位于５７０ｎｍ，表面摩尔吸光度分别为εＣｅ＝３．９６×１０＾６Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，εＳｃ＝４．７１×１０＾５Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，服从比耳定律范围分别为０－２４μｇ／Ｌ Ｃｅ和０－６０μｇ／ＬＳｃ，测定极限为Ｃｅ１．０μｇ／Ｌ（ｎ＝１２）和Ｓｃ１．９μｇ／Ｌ（ｎ＝１０），对     

HPLC determination of diltiazem in human plasma and its application to pharmacokinetics in humans

A simple and sensitive reversed-phase high performance liquid chromatographic method (HPLC) has been developed and validated for the routine analysis of diltiazem in human plasma and the study of the pharmacokinetics of the drug in the human body. Diltiazem and diazepa (internal standard) were extracted with a mixed organic solution of hexane, chloroform and isopropanol (60:40:5, v/v/v), and then HPLC separation of the drugs was performed on an Spherisorb C(18) column and detected by ultraviolet absorbance at 239 nm. The use of methanol-water solution (containing 2.8 mm triethylamine, 80:20, v/v) as the mobile phase at a fl ow-rate of 1.2 mL/min enables the baseline separation of the drugs free from interferences with isocratic elution. The method was linear in the clinical range 0-300 ng/mL and the lower limit of detection of diltiazem in plasma was 3 ng/mL. The range of percentage of relative standard deviation (%RSD) was from 3.5 to 6.8% for within-day analyses and from 6.2 to 8.4% for between-day analyses, respectively. The extraction recoveries of diltiazem from spiked human plasma (n = 5) at three concentrations were 91.4-104.0%. The method has been used to determine diltiazem in human plasma samples from eight volunteers who had taken diltiazem hydrochloride slow release tables and the data obtained was fitted with a program on computer to study the pharmacokinetics. The results showed that the peak level in plasma approximately averaged 118.5 +/- 14.3 ng/mL at 3.1 +/- 0.4 h, and the areas under the drug concentration curves (AUC) was 793.1 +/- 83.1 ng.h/mL.     

Pharmacokinetic study of puerarin in rat serum by liquid chromatography tandem mass spectrometry

A highly sensitive and specific atmospheric pressure chemical ionization liquid chromatography-tandem mass spectrometry method was developed for serum pharmacokinetic studies of puerarin in rats. Chromatography was carried out on a reversed-phase Phenomenex Synergi 4 microm Fusion-RP80 column (150 x 2.0 mm i.d.) using a mobile phase consisting of acetonitrile-water (10:90, v/v) in 10 mm NH(4)OAc with a flow rate of 0.2 mL/min. Puerarin was analyzed in the multiple reaction monitoring mode with a precursor/product ion transition of m/z 415/267. The method was demonstrated to be specific and sensitive, and a linear response was observed over a range of 2-5000 ng/mL in rat serum. The validated method was successfully applied to the characterization of the pharmacokinetics of puerarin in rat serum after oral administration to spontaneously hypertensive rats. The blood concentration-time profile of puerarin showed a rapid initial increase, reaching a maximum and then declining within 1 h. Puerarin could not be detected after 24 h. The main pharmacokinetic parameters for puerarin after oral administration were as follows: C(max) (3.54 +/- 2.03 mg/L), T(max) (0.68 +/- 0.37 h), AUC(0-t) (7.29 +/- 3.79 mg h/L), AUC(0-infinity) (9.17 +/- 4.87 mg h/L), T(1/2) (1.7 +/- 0.6 h), CL/F (7.24 +/- 4.27 L/h/kg) and V/F (17.88 +/- 13.55 L/h/kg).     

Development of an HPLC method for the determination of salidroside in beagle dog plasma after administration of salidroside injection: application to a pharmacokinetics study

A simple RP-HPLC method was established for the determination of salidroside in dog plasma. Salidroside is one of the most active ingredients of Rhodiola L. The method had within-run precision values in the range of +/- 2.3 to +/- 9.1% (n = 5) and between-run precision in the range of +/- 3.2 to +/- 9.8%. A simple protein precipitation for salidroside extraction was processed using ACN at precipitant-to-plasma volume ratio (P-P ratio) of 3:2. The extraction recoveries of salidroside at seven concentrations were higher than 63.2%. There was a linear relationship between chromatographic area and concentration over the range of 0.83-520 microg/mL for salidroside in plasma (R = 0.9926). The LOQ (S/N = 10) of the method was 0.83 microg/mL. The method was applied in a study of the pharmacokinetics of salidroside injection in six beagle dogs. The major pharmacokinetic parameters of C(max), AUC(0-24), AUC(0-infinity), and t(1/2) of salidroside in beagle dogs after i.v. administration of a single 75 mg/kg (5 mL/kg) dose were 96.16 +/- 8.59 microg/mL, 180.3 +/- 30.6 microg h/mL, 189.3 +/- 32.1 microg h/mL, and 2.006 +/- 0.615 h, respectively.     

Ion-pair reversed-phase HPLC method for determination of sodium tanshinone IIA sulfonate in biological samples and its pharmacokinetics and biodistribution in mice

The ion-pair reversed-phase HPLC method for determination of sodium tanshinone IIA sulfonate (STS) in various biological samples was for the first time developed and validated, and was applied for pharmacokinetics and tissue distribution studies of intravenously administrated STS in mice. A linear relation was found between peak area and STS concentrations within the ranges of 0.1-5 micraog/ml for plasma, 0.1-5 microg/g of tissue for kidney homogenate, 0.1-20 microg/g of tissue for liver homogenate, 0.1-1 microg/g of tissue for heart, spleen and lung homogenates, respectively. In plasma and tissues, the limit of quantification (LOQ) and the limit of detection (LOD) for STS were 100 ng/ml and 20 ng/ml. In all biological specimens, the average inter- and intra-day precision of STS were within 4.9%. The recoveries were more than 92% at all concentration levels in each type of biological specimens. STS plasma concentration-time data were best fitted with a two-compartment model, characterized by an initial rapid phase of drug concentration decrease, and a slower terminal elimination phase. The pharmacokinetics of STS was characterized with a distribution half-life (t(1/2alpha)) of 1.2+/-0.18 min, a terminal half-life (t(1/2beta)) of 21.6+/-2.4 min, a distribution volume (V) of 0.057+/-0.011 l/kg, a plasma clearance (CL) of 0.86+/-0.12 l/h/kg and an AUC(0-infinity) of 58.41+/-6.21 microg x h/ml. STS was widely distributed into most tissues and was obviously accumulated in liver. This results indicated that STS may be promising to treat liver disease.     

HPLC determination of andrographolide in rat whole blood: study on the pharmacokinetics of andrographolide incorporated in liposomes and tablets

A sensitive and simple high-performance liquid chromatographic method with UV detection was developed and validated for the determination of andrographolide in rat whole blood. Carbamazepine was employed as internal standard and the blood sample was extracted with chloroform. Chromatographic separations were achieved on a Chromasil ODS column (250 x 4.6 mm, 5 microm). The mobile phase was consisted of methanol-water (52:48, v/v) and delivered at 0.8 mL/min. The detection wavelength was set at 225 nm. The calibration curve had a good linearity in the range 0.053-530 microg/mL in rat whole blood with its correlation coefficient being 0.996. The extraction recovery of andrographolide was ranged from 65.7 to 72.6%. The intra-day and inter-days repeatabilities were below 4.2% in terms of the percentage of relative standard deviation (RSD). The method was used to provide data on the pharmacokinetics of the drug in rats. The data obtained was processed using the 3P87 pharmacokinetic program. The results showed that the disposition of andrographolide after intravenous administration of liposomal andrographolide conformed to a two-compartment open model with alpha = 4.75 x 10(-2) +/- 2.41 x 10(-3) min(-1), beta = 3.16 x 10(-3) +/- 1.58 x 10(-4) min(-1), V(c) = 174.67 +/- 13.97 mL, k(21) = 1.60 x 10(-2) +/- 8.12 x 10(-4) min(-1), k(10) = 9.38 x 10(-3) +/- 5.62 x 10(-4) min(-1), k(12) = 2.53 x 10(-2) +/- 1.27 x 10(-3) min(-1) and AUC(0-infinity) = 1525.47 +/- 92.35 microg min/mL. For the intragastric administration of andrographolide tablets, the disposition of andrographolide followed a one-compartment open model with k(e) = 6.78 x 10(-3) +/- 3.53 x 10(-4) min(-1), k(a) = 3.69 x 10(-2) +/- 4.68 x 10(-3) min(-1), T(max) = 59.69 +/- 3.61 min, C(max) = 1.62 +/- 0.11 microg/mL, V(c) = 1056.90 +/- 83.42 mL, AUC(0-infinity) = 348.75 +/- 24.41 microg min/mL.     

Cathodic adsorptive stripping square-wave voltammetric determination of nifedipine drug in bulk,pharmaceutical formulation and human serum

Nifedipine is a calcium-channel antagonist drug used in the management of angina pectoris and hypertension through inhibition of calcium influx. A fully validated sensitive cathodic adsorptive stripping square-wave voltammetry procedure was optimized for the determination of the drug at trace levels. The procedure was based on the reduction of the nitrophenyl group after the interfacial accumulation of the drug onto a hanging mercury drop electrode in Britton-Robinson buffer of pH 11.0. The optimal conditions of the procedure were found to be: accumulation potential=-0.9 V vs. Ag/AgCl/KCl(s)), accumulation time=30 s, scan increment=10 mV, pulse amplitude=50 mV and frequency=120 Hz. Under these conditions, a well-defined peak was obtained; its peak current showed a linear dependence on drug concentration in the range of 2x10(-9)-2x10(-7) mol L(-1) bulk nifedipine. The mean recoveries based on eight replicate measurements for 1x10(-8) and 5x10(-8) mol L(-1) bulk nifedipine solutions were 98.46+/-0.86% and 98.23+/-0.92%, respectively. A detection limit of 3.42x10(-10) mol L(-1) bulk nifedipine was achieved. The procedure was successfully applied for assay of the drug in tablets and spiked human serum with mean recoveries of 101.95+/-1.42% and 98.70+/-0.63%, respectively. The limit of detection of the drug in spiked human serum was found to be 3.90x10(-10) mol L(-1).     

HPLC analysis and pharmacokinetics of icariin in rats

As a prerequisite to the determination of pharmacokinetic parameters of icariin in rats, an HPLC method using UV detection was developed and validated. Icariin and the internal standard, quercetin, were extracted from plasma samples using ethyl acetate after acidification with 0.05 mol/L NaH2PO4 solution (pH 5.0). Chromatographic separation was achieved on an Agilent XDB Cls column (250 x 4.6 mm id, 5 microm) equipped with a Shim-pack GVP-ODS C18 guard column (10 x 4.6 mm id, 5 microm) using a mobile phase of ACN/water/acetic acid (31:69:0.4 v/v/v) at a flow rate of 1.0 mL/ min. Detection was at 277 nm. The calibration curve was linear from 0.05 to 100.0 microg/mL with 0.05 microg/mL as the lower LOQ (LLOQ) in plasma. The intra- and interday precisions in terms of RSD were lower than 5.7 and 7.8% in rat plasma, respectively. The accuracy in terms of relative error (RE) ranged from -1.6 to 3.2%. The extraction recoveries of icariin and quercetin were 87.6 and 80.1%, respectively. The main pharmacokinetic parameters for rats were determined after a single intravenous administration of 10 mg/kg icariin: t1/2, 0.562 +/- 0.200 h; AUC0-infinity, 8.73 +/- 2.23 microg x h/mL; CLToT, 20.10 +/- 5.80 L/kg x h; Vz, 1.037 +/- 0.631 L/kg; MRT0-infinity, 0.134 +/- 0.040 h; and Vss, 0.170 +/- 0.097 L/kg.     

反相高效液相色谱法测定肾舒冲剂水煎液中的小檗碱

 :应用反相高效液相色谱法检测了肾舒冲剂水煎液中的小檗碱。样品经超声提取后,以C18化学键合硅胶为固定相,乙腈-0.04mol/LH3PO4(体积比为42∶58)为流动相,用349nm的波长定量检测。测定结果表明,小檗碱的质量浓度在1.2～19.2mg/L范围内线性良好,最低检测限为0.6mg/L,测定批内(n=5)及批间(n=5)相对标准偏差分别为0.6%～3.5%和5.3%～6.5%,回收率为89.10%～91.35%。     

Determination of total arsenic in serum and packed cellsof patients with renal insufficiency

In order to investigate the arsenic level in serum and packed cells of patients with renal insufficiency, total arsenic (As) concentrations were determined with hydride generation atomic absorption spectrometry (HGAAS) in serum (S) and packed cells (PC) of 31 non-dialyzed patients. The accuracy of the method was tested by the analysis of arsenic in 3 certified reference materials. Patients showed a three-fold increase of arsenic concentrations in serum and a two-fold increase of arsenic in packed cells compared with controls. Patients (n=10) with higher serum creatinine (>2.0 mg/dL), urea (>0.70 g/L) and urinary protein (mean+/-SD: 1.12+/-0.82 g/L) showed higher arsenic concentrations (5.8+/-3.3 microg/L in serum and 18.0+/-16.7 microg/kg in packed cells) compared with those with lower creatinine (<1.6 mg/dL), urea (<0.6 g/L) and urinary protein (mean+/-SD: 0.27+/-0.82 g/L) (n=16, serum arsenic 1.2+/-1.2 microg/L, packed cells arsenic 2.6+/-1.9 microg/kg). The significant differences (both p < 0.001) in S and PC-arsenic levels of patients in group I and II implies a relationship between the arsenic level and the degree of chronic renal insufficiency.     

高效液相色谱法测定大鼠血浆中的原儿茶酸

建立了大鼠血浆中原儿茶酸含量测定的高效液相色谱方法。采用的色谱柱为DiamondsilTM C18 柱(150 mm×4.6 mm,5 μm);流动相为乙腈-水(体积比为9∶91,用H3PO4 调pH至2.5);流速1.2 mL/min;检测波长260 nm;内标为对羟基苯甲酸。原儿茶酸的线性范围为0.050~3.20 mg/L,线性相关系数为0.9978，最低定量限为0.050 mg/L,日内和日间测定的精密度（以相对标准偏差表示）均低于7.0%,准确度（以相对误差表示）为-1.4%～2.6%；在0.050,0.40,3.20 mg/L低、中、高3个添加浓度水平下，血浆样品的提取回收率分别为83.4%,87.3%,91.1%。该方法简便,灵敏,准确,适用于大鼠体内原儿茶酸的药物动力学研究。