High Performance Liquid Chromato-Graphic Method For The Determination Of Permethrin Deposits In A Forestry Spray Trial

Abstract

A convenient and sensitive reversed-phase high performance liquid Chromatographie method has been developed for the determination of perraethrin [3-phenoxybenzyl (±)- cis,trans -3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropanecarboxylate] insecticide. Various isocratic and gradient mobile phases, consisting of acetonitrile:water (CH₃CN:H₂O) and methanol:water (CH₃OH:H₂O) solvent systems at two flow rates, were tested to separate and quantify the Isoners of permethrin using octadecylsilyl (ODS) (Regis 5μ m) and octylsilyl (OS) (RP-8, 10 μ m) bonded columns. The optimal mobile phase for perraethrin using the ODS column was 70:30 (v/v) CH₃CN:H₂O mixture at flow rates of either 1.0 or 1.5 mL/min. The measurement was done with a UV detector at 200 nm and 50°C. The OS column gave a less satisfactory separation than the ODS. Gradient elution systems examined did not improve the iso-meric separation of perraethrin. Using the method developed, deposit levels obtained on various sampling units during a perraethrin spray trial were analyzed after elution or extraction followed by necessary column cleanup. Minimum levels of detection for permethrin varied from 1 to 3 ng depending on the nature of the sampler used.     

测定兔血清中氟尿嘧啶的高效液相色谱法

改进了血清中氟尿嘧啶的液相色谱分析方法 ,采用DiamonsilC18150mm×4.6mm×5μm分析柱 ,ODS50mm×4.6mm×10μm为保护柱 ,UV检测波长为270nm ,甲醇 -水(体积比3∶97 ,冰醋酸调pH=3.5)为流动相 ,流速0.5mL·min-1,外标法定量 ;以乙酸乙酯萃取血浆样品 ;氟尿嘧啶在0.17～42.50mg·L-1 范围内线性良好 ,日间RSD(n=5)为1.9%～2.3 %,日内RSD(n=5)为0.9 %～1.0 % ,方法回收率为92 % ;该法准确 ,适用于氟尿嘧啶常规监测及药代动力学研究     

高效液相色谱法测定人血清中5-氟尿嘧啶浓度

建立了测定人血清中5-氟尿嘧啶的反相高效液相色谱法。采用ZorbaxODS柱4.6mm×250mm,预柱YWG-C184.6mm×50mm;甲醇:水（20:80）为流动相,紫外检测波长为273um,喃氟啶为内标定量。回收率为96.85％,田间和日内变异系数分别为537％和438％,血清中最低检测浓度为10μg／L。在0.04～50mg／L浓度范围内线性良好,相关系数为0.9990。     

High Pressure Liquid Chromato-Graphic Separation of Aryl-Naphthalide Lignan Lactones

Abstract

A high-pressure liquid chromatographic system is described for the separation of few arylnaphthalide lignan lactones. An octadecyl-silica (Spherisorb 5 ODS) column was used with methanol/water (73/27 volume %) isocratic system as eluent. Both HPLC-fluorometry and HPLC-UV detection methods were employed. The present technique is compared with other instrumental methods developed earlier and its utility in chemotaxonomic and toxicologic studies is discussed.     

High Performance Liquid Chromatographic Assay of Phenacemide in Tablets

Abstract

A rapid, specific and reliable high-performance liquid chromatographic assay of phenacemide in tablets has been developed. Reversed-phase chromatography was conducted using a mobile phase of acetonitrile and acetate buffer, pH 4.2 (50% V/V) and detection at 254 nm. The recovery and coefficient of variation from six placebo samples of 100 mg were 100.2% and 0.57%, respectively. The percent recovery of 10 replicate commercial tablets was 101.1% of the label amount and its coefficient of variation was 0.95%. Regression analyses of three standard plots in the concentration range of 15-150 μ g/ml obtained on three different days gave a correlation coefficient > 0.999 and the coefficient of variation for their slopes <2%. The HPLC method is rapid as it takes - 1 hour to analyze six commercial tablets compared with 6 hours consumed by the USP method. The assay was precise within day and between days as indicated by ANOVA test.     

High Performance Liquid Chromatographic Assay of Hydromorphone Hydrochloride Injection

Abstract

A stability indicating high performance liquid chromatographic (HPLC) method for determining hydromorphone hydrochloride in dosage forms is described. The drug was chromatographed on a C₁₈ reverse phase column, using a mobile phase consisting of sodium lauryl sulfate, acetic acid, acetonitrile and water, and detected at 280 nm. Linearity of detector response to the concentration was confirmed. The procedure showed excellent reproducibility and gave quantitative recoveries of the drug from spiked placebos. Photodegraded samples of the dosage form, were assayed by the HPLC procedure and the current USP spectrophotometric procedure. Comparison of the results showed that the USP procedure is only partially stability indicating.     

小鼠组织中肝靶向前药5-氟尿嘧啶含量的高效液相色谱法测定

以5-溴尿嘧啶为内标,建立了高效液相色谱法测定小鼠组织中肝靶向前药(半乳糖化人血清白蛋白与5-氟尿嘧啶偶联物)中5-氟尿嘧啶(5-FU)含量的分析方法.样品经盐酸水解、乙酸乙酯提取、离心后,取上清液在40 ℃下用N2吹干,用流动相溶解、定容后进样分析.色谱条件:安捷伦Hypersil C18色谱柱(4.0 mm×250 mm, 5 μm),流动相为甲醇-磷酸缓冲溶液,流速0.7 mL/min,UV检测波长为270 nm.方法的线性范围为1 ～20 mg/L,检出限(S/N=3)为0.1 mg/L,回收率为93% ～104%.该法操作简便、灵敏度高,适于组织中肝靶向前药半乳糖化人血清白蛋白与5-氟尿嘧啶偶联物(Gal-HSA-5-FU)的5-FU含量测定.     

Assay of Brain Tocopherols Using High Performance Liquid Chromatography

Abstract

The four natural tocopherols were separated using a μ-Bondapak-NH₂ column. For the analysis of brain tocopherols 5,7-dimethyltocol was used as an internal standard. α-Tocopherylquinone and other tocopherols than α-tocopherol were not detected. Rat cerebral cortex and cerebellum contained 19.3 μmol/g and 11.2 μmol/g of α-tocopherol, respectively. A chromatographic system with a reversed-phase column proved less suitable.     

Rapid Assay of Hypothalamic Aromatase Using High Performance Liquid Chromatography

Abstract

A rapid assay for hypothalamic aromatase has been developed using HPLC. Each assay tube contained rat anterior hypothalamus homogenized in Na phosphate buffer (pH 7.0), NADPH regenerating system, unlabelled estradiol and estrone, and 10 μCi of ³H-androstenedione. After agitation at 37°C for 3 hours, the reaction mixture was extracted with CH₂Cl₂, partitioned between 90% methanol and hexane, and the methanol layer chromatographed on a Waters 10μ C-18 Radial-PAK column using acetonitrile/water (70:30). The estrogens were collected together and rechromatographed with THF/water (35:65). The estrone peak was collected, and the ³H-estrone produced was determined by liquid scintillation. The estrone collected from the second chromatographic step was found to be at least 95% pure by methylation and rechromatography. Using the HPLC procedure, enzymatic ³H-estrone formation was found to be linear in a time and protein dependant manner.     

High Performance Liquid Chromatography Assay of Itraconazole in Human Plasma

Abstract

A high performance chromatographic method, using internal standard quantification, for the analysis of Itraconazole in human plasma is described. The standard curve was linear over the concentration range tested. The detection limit of the method was 250 ng. An authentic sample of both Itraconazole and the internal standard (ketoconazole) were used to establish the calibration curve.     

Salsolinol合成酶的高效液相色谱-电化学活性检测方法研究

Salsolinol合成酶是一种催化多巴胺(DA)和乙醛(AcH)生成Salsolinol的酶,它在内源性儿茶酚异喹啉类物质代谢过程中起重要作用。研究显示该类物质具有一定的神经毒性,与帕金森病(PD)发病机制密切相关,因此Salsolinol合成酶可能是PD的一种关键致病因子。本文从雄性SD大鼠鼠脑中分离得到Salsolinol合成酶的粗酶液,采用高效液相色谱结合电化学检测器体系(HPLC-ECD)建立了一套灵敏度高、重复性较好的酶活检测方法,并进行了方法稳定性和灵敏度的验证,方法简便、稳定,适用于不同生物样品中该酶活性的测定;同时也将该方法应用于超滤分离后不同截留分子量样品的活性测定,结果显示该酶的活性主要集中在3K下层滤液。     

High Performance Liquid Chromatographic Assay of phenylbutazone in Pharmaceutical Dosage Forms

Abstract

A simple, rapid and reliable high performance liquid chromatographic procedure for the quantitation of phenylbutazone in pharmaceutical dosage forms was developed, and compared with the U. S. P. XXI method and a spectrophotometric assay developed in this laboratory. A comparison of the three methods indicated that the HPLC method is the most rapid, simple and reproducible. The recoveries based on six placebo samples were 100.2, 99.2, and 99.4% by HPLC, UV and the U. S. P. method, respectively, and their respective CVs were 0.39, 0.73, and 1.5%. Replicate regression analyses of three standard plots in the concentration range of 0.02-0.12 mg/ml obtained using the HPLC assay on three different days yielded a correlation coefficient <0.999 and the coefficient of variation for the three slopes was 1.05%. It is suggested that the proposed HPLC method should be used for routine quality control and dosage form assay of phenylbutazone.     

High Performance Liquid Chromatographic Assay of Verapamil Hydrochloride in Dosage Formsk

Abstract

A stability indicating high-performance liquid chromatographic (HPLC) method for determining verapamil hydrochloride in dosage forms is described. The assay affords baseline separation of the drug from its synthesis impurities and from photolytic degradation products, as well as from formulation excipients. The drug was extracted in 0.05 N hydrochloric acid, chromatographed on a C₁₈ reverse-phase column, eluted with methanol-water-acetic acid-triethylamine (55:44:1:0.1) and the effluent was detected at 280 nm. Linearity studies were carried out using peak height or peak area measurements and the detector response to the concentration of verapamil hydrochloride was confirmed. Excellent interlaboratory precision and recovery data were obtained by the spiked placebo method. This procedure was rapid and selective for the assay of the cardiotonic drug. Application of the method for the assay of verapamil hydrochloride in representative dosage forms is described.     

Assay of Arginine-Esterase Activities by Reversed Phase High Performance Liquid Chromatography

Abstract

Application of a high performance liquid chromato-graphic technique to assay of arginine-esterase activities is presented. Enzyme reaction was carried out with benzoyl-L-arginine ethylester as a substrate and analysis was performed on a reversed phase chromato-graphic system using a μ Bondapak C₁₈ or a Radial-PAK A column and buffered aqueous methanol as the mobile phase. The enzyme activities were determined by the peak height of cleaved product (benzoyl-L-arginine). The minimum detection limit for benzoyl-L-arginine was 0.02 nM on each column. The generality of this method was demonstrated by its application to determination of plasmin activity, and so it might be suitable for both kinetic studies and routine assays of plasmin-like es-terases.     

反相离子对高效液相色谱法测定大白鼠牙髓中5－羟色胺

A high performance liquid chromatographic method with electrochemical detection for measuring 5-hy-droxytryptamine(5-HT) in the dental pulp of white rat is presented in the paper.Protein was precipitated by3.3%trichloroacetic acid and 200μL of supernatant was injected.Chromatography was performed on aYWG-C(18) column. Isoproterenol was used as internal standard.The calibration curve was linear within therange of 0. 125～2ng/mL.     

返魂草的高效液相色谱法指纹图谱研究及成分分析

采用高效液相色谱法,建立了返魂草的指纹图谱,并与相同条件下获得的同属植物千里光图谱进行了比较;通过液相色谱-质谱联用法及与对照品比照研究,对其5种共有成分进行了鉴定;并对以上成分的含量进行同步测定。结果表明,此指纹图谱能够用于区分返魂草及其混淆品千里光;5种成分在各自的浓度范围内线性关系良好(r=0.9995～0.9998),10批样品中原儿茶酸、绿原酸、咖啡酸、金丝桃苷、异槲皮苷含量分别为0.03～0.07 mg/g,0.10～1.04 mg/g,0.01～0.05 mg/g,0.07～0.35 mg/g和0.02～0.74 mg/g。本方法可用于返魂草的鉴别及药材的质量评价。     

High Performance Liquid Chromatographic Assay for Adinazolam Mesylate in Rodent Feed Mixtures

Abstract

Adinazolam mesylate was recovered from the feed mixtures by repeated extraction with a pH 4 citrate buffer. The pooled extracts were diluted with water when necessary and mixed with an equal volume of an acetonitrile solution of internal standard (naphthalene). After mixing and centrifugation, the clear supernates were separated for chromatography. The chromatography was carried out on a reverse phase column using a mixture of phosphate buffer, acetonitrile and methanol in the volume ratios of 85:40:20 as mobile phase. Adinazolam and the internal standard were eluted from the columns at about 11.7–12 and 15.50–17.5 minutes, respectively.

The peak height ratios and adinazolam mesylate concentrations showed excellent linearity (r>0.999). Extracts of blank feed samples did not show interference to the assay. Assay results with satisfactory accuracy and precision were obtained. The methodology was applicable for the assay of the drug-feed mixtures containing 0.02 to 10.0 mg of adinazolam mesylate per gm of feed.     

A New High Performance Liquid Chromatographic Assay for Fluspirilene in Dosage Forms

Abstract

A new method for the assay of fluspirilene (R 6218) in dosage forms using HPLC has been developed. The instrument used had a low volume positive displacement pump, a universal injector, a single wavelength (254 nm) detector, and a data module. The column was stainless steel 30 cm × 4 mm i.d. packed with microparticulate silica. The mobile phase consisted of equal volumes of chloroform and methanol at a flow rate of 1 ml per min. A linear relationship (r = 0.999) was obtained between peak area and concentration of fluspirilene in the range 10–200 μg per ml; no internal standard was used. Fluspirilene was extracted from injectable aqueous suspensions by membrane filtration, drying and dissolution in chloroform-methanol (1:1). Results of assaying fluspirilene in two commercial injectable suspensions by this method were 99.73 and 99.78% of labelled amount.     

A New Assay for Argininosuccinate in Urine Samples by High Performance Liquid Chromatography

Abstract

A rapid, sensitive and simple procedure has been developed for determination of argininosuccinate (ASA). The assay is based upon the enzymatic cleavage of ASA in the presence of excess of argininosuccinate lyase (ASAL), HPLC separation and UV-detection of fumarate formed. The calibration curve, obtained using standards, derives from a linear correlation between the reaction rate and ASA concentration. The range of HPLC detection corresponds with the level of normal excretion of argininosuccinate in urine from the patients with argininosuccinate lyase deficiency (ASLD).     

A Stability Indicating High Performance Liquid Chromatographic Assay of Isradipine in Pharmaceutical Preparations

Abstract

A high performance liquid chromatographic procedure has been developed for the assay of isradipine in bulk form and tablet and capsule pharmaceutical preparations. The separation is achieved within 20 min on an octadecylsilane column at ambient temperature with a mobile phase of 60:40 v/v methanol - water, a flow rate of 1 mL/min, and detection at 325 nm. Degradation studies showed no peak interference between isradipine and degradation products. It was also determined that the excipients in the commercial tablet and capsule preparations did not interfere with the assay. The method was linear in the range 10–60 μg/mL with accuracy and precision in the 0.40 - 1.53% range.