杆菌肽脂质体的制备及其药物含量测定

目的：制备杆菌肽脂质体,并采用HPLC法测定杆菌肽脂质体中杆菌肽含量和包封率。方法用薄膜分散法将杆菌肽制备成杆菌肽脂质体;色谱条件：色谱柱为Diamonsil-C18色谱柱（150mm×4.6mm,5μm）;流动相为pH 6.0的磷酸盐缓冲液-甲醇（60∶40）;柱温为25℃;检测波长为254nm;流速为1mL/min。采用低温离心法分离杆菌肽脂质体中的游离药物。结果所制备的杆菌肽脂质体的平均包封率为87.94%（RSD 1.12%, n=5）;在本色谱条件下,杆菌肽在0.061~1.83μg范围内与峰面积积分值的线性关系良好（R2=0.9997）,平均回收率为99.68%~101.38%。结论本HPLC法简单,准确可靠,可用于杆菌肽脂质体中杆菌肽含量及其包封率的测定。     

The determination of nadolol in biological samples using high-performance liquid chromatography

A method has been developed for the determination of nadolol in biological samples by reversed-phase high-performance liquid chromatography with fluorimetric detection. The method has been applied to plasma, serum and urine samples, which are prepared by extraction with diethyl ether-dichloromethane (5:2,v/v), evaporation of the organic solvent, and dissolution of the resultant residue in the chromatographic eluent. The sample is then subjected to chromatography on a C(18)-silica column, with an eluent of water-acetonitrile-triethylamine (800:200:1,v/v) adjusted to pH 3.0 with orthophosphoric acid. A single point external standard is used for quantitation. The working ranges were 1-400 ng/ml for plasma/serum, and 0.1-40 mug/ml for urine, although a detection limit of 0.1 ng/ml appears to be readily attainable. The sample size was 0.5 ml, and for both types of sample the method showed good correlation with a previously published fluorimetric method (for plasma, r = 0.9544, n = 70; for urine, r = 0.9919, n = 35).     

丝裂霉素加凝血酶胸腔注入治疗癌性胸腔积液临床观察

本文对用丝裂霉素及凝血酶联合胸腔注入治疗癌性血性胸水进行了对比,对照组14例：胸腔抽液后注入丝裂霉素8mg，实验组14例：在胸腔抽液后注入丝裂霉素8mg及凝血酶2000u；结果显示实验组疗效显著高于对照组（P＜0．01），提示用丝裂霉素及凝血酶联合治疗癌性血性胸腔积液是一种有效治疗方法。     

Comparison of zero- and second-order derivative spectrophotometric and HPLC methods for the determination of gemcitabine in human plasma

Zero- and second-order derivative spectrophotometric and high-performance liquid chromatography (HPLC) methods were developed and validated for the determination of gemcitabine in human plasma. Spectrophotometrically, gemcitabine was determined by means of zero-order derivative absorbance values (A) at 288 nm and from values from the second-order derivative absorbance values (2D) at 285 nm. Beer's Law was obeyed in the range 0.50-15.0 microg ml(-1). The proposed other method, normal-phase HPLC method for determination of gemcitabine in human plasma was described. Calibration curve was linear over the concentration range 0.20-15.0 microg ml(-1). Quantitation was achieved by diode array detection at 272 nm using 2'-deoxycytidine as internal standard. Results obtained by spectrophotometric and HPLC methods for determination of gemcitabine in human plasma described in this paper showed adequate accuracy, precision and repeatability. No interference was found in plasma at the selected derivative wavelength and chromatographic conditions. According to the statistical comparison, there is no significant difference between the three methods. This is suggested that the three methods are equally applicable.     

白细胞介素2与丝裂霉素联合胸腔注入治疗晚期肺癌癌性胸腔积液的效果观察

本文对用白细胞介素2及丝裂霉素以及两药联合胸腔注入治疗癌性胸水进行了对比,每组9例病人。两药联合胸腔注入治疗9例病人中7例有显著疗效,优于单一药物胸腔注入治疗。两种药物有一定减少癌性胸水渗出增长的作用,联合胸腔注入治疗晚期肺癌癌性胸腔积液作为一种新方法安全、有效。     

Simultaneous HPLC determination of nitrendipine and impurities of the process of synthesis

A method has been developed for separation of nitrendipine and its impurities of reaction partners and side reaction products by high-performance liquid chromatographic method on a RP-18 column and detection at 238 nm. The mobile phase composition that provided an acceptable nitrendipine resolution, in large excess and possible impurities, in a short elution time, is methanol:water (70:30) and pH 3. Linearity (r≥0.999), reproducibility (RSD=0.8–1.4%), determination limit (0.5–2%) and recovery (99.8–102.3) were validated and found to be satisfactory. This method enables monitoring of the process of synthesis, as well as the choice of the synthetic design.     

Simple high-performance liquid chromatographic method for the determination of acyclovir in pharmaceuticals

An assay method for the determination of acyclovir from pharmaceutical preparations has been developed for assessment of product quality utilising high-performance liquid chromatography. The chromatographic conditions comprised a reversed-phase C18 column (250 x 4.6 mm i.d.) with a mobile phase of acetonitrile-20 mmol l(-1) aqueous ammonium acetate buffer of pH 4.5 (40:60). The flow rate was 0.8 ml min(-1) and UV detection was used at 250 nm. Calibration graph was linear in the range 1.98-59.4 microg ml(-1). The method has been validated according to current guidelines including assay of pharmacopoeial standard tablets. Recoveries ranged from 96.64 to 99.53%. The exipients present in the tablets did not interfere with the method.     

Simultaneous determination of p-aminobenzoic acid and its metabolites in the urine of volunteers, treated with p-aminobenzoic acid sunscreen formulation

p-Aminobenzoic acid (PABA) and its metabolites (p-aminohippuric acid, p-acetamidobenzoic acid, and p-acetamidohippuric acid) were detected using high-performance liquid chromatography with an electrochemical (carbon paste) detector (HPLC-ECD). For direct current (dc) mode, with the current at a constant potential, and measurements with suitable experimental parameters, a linear concentration from 0.125 to 1.80 microg/ml was found. The detection limit was approximately 2.0 ng/ml. A carbon paste coulometric detector was used to demonstrate that PABA and its metabolites are electrochemically oxidized in acidic media, and to determine, by analyzing human urine, the percutaneous absorption of PABA and its metabolites. Findings using HPLC-ECD and HPLC with an ultraviolet detector (HPLC-UV) were comparable.     

A high-performance liquid chromatographic method for the determination of stobadin pharmacokinetics in serum

A high-performance liquid chromatographic method was developed to determine stobadin pharmacokinetics in dog and man. The relative bioavailability of stobadin dipalmitate compared with dihydrochloride was 46.4 per cent in dog. In man peak serum concentrations ranged from 12 to 289 ng ml-1 after a single oral dose of stobadin dipalmitate (0.79 to 2.5 mgkg-1).     

Packed capillary liquid chromatography coupled to fluorescence detection: Application to human blood samples for the determination of glutathione

The present investigation analyses the potentials of capillary chromatography using packed fused silica capillaries filled with 5 microns RP-18 for the fluorescence determination of glutathione in human blood samples. Adaptation of conventional HPLC equipment for miniaturized chromatographic assays proved successful. Sample preparation was relatively simple, though care should be taken in sample handling. The thiolic compound mercaptoethanol was used as internal standard. Qualitative determinations were based on standard addition providing increased peak heights at identical retention times. Quantitative determinations gave linear calibration curves, with a standard glutathione recovery of 98.9% and an intra-assay reproducibility of 3.3%. The glutathione values measured appeared within the normal range of 0.9-1.7 mmol glutathione per litre of blood.     

HPLC-MS/MS法同时检测生物样本中的氯霉素、甲砜霉素及氟甲砜霉素

目的 建立专属灵敏的高效液相色谱-质谱法( HPLC-MS/MS),用于生物样本中的3种常见抗生素氯霉素、甲砜霉素及氟甲砜霉素的微量检测.方法 生物样本(猪肉、猪肝)经一定的方法提取并纯化后,采用高效液相色谱分离3种抗生素,并用电喷雾离子化串联质谱( ESI-MS/MS)进行检测和定量分析.结果 氯霉素在0.1～10 ng·mL-1、甲砜霉素及氟甲砜霉素在10～100 ng·mL-1线性关系良好,回收率＞86％,RSD＜10％.结论 该方法灵敏度高、专属性强,回收率较高、精密度较好,适用于生物样本中的微量氯霉素、甲砜霉素及氟甲砜霉素的检测.     

一种简易测定人血浆氧氟沙星浓度的高效液相色谱法

目的　建立一种简易的测定人血浆氧氟沙星浓度高效液相色谱法。方法　血浆由蛋白沉淀剂[甲醇∶ 5 % Zn SO4 (70∶ 30 ,v/v) ]沉淀蛋白后上清液直接进样。所用色谱柱为 Hypersil BDS C1 8柱 ,流动相为0 .0 5 mol/L 柠檬酸缓冲液 (三乙胺调 p H值到 4 .0 )∶乙腈 (83∶ 17,v/v) ,荧光检测器激发波长为 2 95 nm,发射波长为 5 0 5 nm。结果　直接沉淀蛋白后样品干净 ,色谱分离效果好 ,无内源性杂质干扰。在 0 .0 1～ 15 μg/ml浓度范围内线性关系好。提取回收率为 76 .3% ,日内精密度和日间精密度均小于 10 %。结论　本法简便、可靠 ,可用于血药浓度测定。     

A validated HPTLC method for determination of terbutaline sulfate in biological samples: Application to pharmacokinetic study

Terbutaline sulfate (TBS) was assayed in biological samples by validated HPTLC method. Densitometric analysis of TBS was carried out at 366 nm on precoated TLC aluminum plates with silica gel 60F₂₅₄ as a stationary phase and chloroform–methanol (9.0:1.0, v/v) as a mobile phase. TBS was well resolved at R_F 0.34 ± 0.02. In all matrices, the calibration curve appeared linear (r² ⩾ 0.9943) in the tested range of 100–1000 ng spot⁻¹ with a limit of quantification of 18.35 ng spot⁻¹. Drug recovery from biological fluids averaged ⩾95.92%. In both matrices, rapid degradation of drug favored and the T_0.5 of drug ranged from 9.92 to 12.41 h at 4 °C and from 6.31 to 9.13 h at 20 °C. Frozen at −20 °C, this drug was stable for at least 2 months (without losses >10%). The maximum plasma concentration (Cp_max) was found to be 5875.03 ± 114 ng mL⁻¹, which is significantly higher than the maximum saliva concentration (Cs_max, 1501.69 ± 96 ng mL⁻¹). Therefore, the validated method could be used to carry out pharmacokinetic studies of the TBS from novel drug delivery systems.     

Application of ion mobility spectrometry for the determination of tramadol in biological samples

In this study, a simple and rapid ion mobility spectrometry (IMS) method has been described for the determination of tramadol. The operating instrumental parameters that could influence IMS were investigated and optimized (temperature; injection: 220 and IMS cell: 190°C, flow rate; carrier: 300 and drift: 600 mL/minute, voltage; corona: 2300 and drift: 7000 V, pulse width: 100 μs). Under optimum conditions, the calibration curves were linear within two orders of magnitude with R² ≥ 0.998 for the determination of tramadol in human plasma, saliva, serum, and urine samples. The limits of detection and the limits of quantitation were between 0.1 and 0.3 and 0.3 and 1 ng/mL, respectively. The relative standard deviations were between 7.5 and 8.8%. The recovery results (90–103.9%) indicate that the proposed method can be applied for tramadol analysis in different biological samples.     

Direct derivatization of drugs in untreated biological samples for gas chromatographic analysis

The possibilities to derivatize an analyte directly in the biological sample are reviewed with examples from our own experiences and from the literature. Techniques, such as extractive acylation, alkylation and benzoylation, are frequently used. Improvement of the extractability of the drug from the matrix is a common feature, especially with hydrophilic compounds, where sometimes cyclizing reactions can be employed. Several analytes are reactive or labile in the sample and can be trapped in derivatization reactions in situ. In many cases, two-phase reactions lead to milder derivatization conditions (e.g. dealkylation of tertiary amines), which is favourable from a clean-up point of view.     

Validation of a RP-LC method for the simultaneous determination of isoniazid,pyrazinamide and rifampicin in a pharmaceutical formulation

A simple and accurate liquid chromatographic method was developed and validated for estimation of isoniazid (ISN), pyrazinamide (PYR) and rifampicin (RIF) in combined dosage forms. Drugs were chromatographed on a reverse phase C18 column using a mobile phase gradient and monitored at the corresponding maximum of each compounds. Peaks were identified with retention time as compared with standards and confirmed with characteristic spectra using diode-array detector. Solution concentrations were measured on a weight basis to avoid the use of an internal standard. The method does not require any specific sample preparation except the use of a guard column. The method is linear (r²>0.999), precise (RSD%: 0.50% for ISN, 0.12% for PYR and 0.98% for RIF), accurate (overall average recovery yields: 98.55% for ISN, 98.51 for PYR and 98.56% for RIF) and selective. Due to its simplicity and accuracy the method is suitable for routine quality control analysis of antitubercolosis combination dosage form.     

固相萃取HPLC-UV法测定人血浆中比阿培南浓度及其药代动力学研究(英文)

比阿培南是一种新型经胃肠外吸收的碳青霉烯类抗生素,广泛用于治疗多种细菌感染。本试验建立了一种简便、有效、精确的固相萃取HPLC法测定人血浆中比阿培南的浓度。样品和内标物Vitamin B6经固相萃取后通过Capcell Pak C18柱进行分离。测定方法以0.05mol/L磷酸二氢钠(pH5.7)–甲醇(98:2,v/v)为流动相,流速为1.0mL/min,检测波长为300nm。比阿培南在0.04~50.00μg/mL浓度范围内线性关系良好,最低定量限可至0.04μg/mL,0.10、5.00和25.00μg/mL三个浓度的提取回收率均在70%左右。这种测定方法成功地应用于12名健康志愿者单次静脉滴注三剂量(150、300和600mg)比阿培南后的药动学研究。本方法具有良好的精密度和准确度,并且保证样品处理后的稳定性,因此能广泛应用于临床研究。     

维C银翘片中对乙酰氨基酚含量测定方法改进

目的:采用高效液相色谱法(HPLC)测定维C银翘片中对乙酰氨基酚的含量,以避免用双波长分光光度法测定时出现的干扰因素.方法:采用HPLC法,双波长分光光度法分别测定不同批号的维C银翘片中对乙酰氨基酚的含量.结果:双波长分光光度法较繁琐、误差大,HPLC法简便、快速、准确.结论:HPLC法准确可靠,适用于维C银翘片的质量控制.