Topological indices and QSPR analysis of some chemical structures applied for the treatment of heart patients

In this study, various beta-blocker drugs used for heart disease were analyzed, and their degree-based topological indices derived from the M-polynomial were calculated. Linear and quadratic regression analysis was used to obtain quantitative structure-property relationship models between the topological indices and eight the physicochemical properties of the drugs to determine their effectiveness. The results show that the harmonic index was the best predictor for boiling point, flashpoint, and enthalpy of vaporization, while the redefined third Zagreb index was effective for polarizability, molar refractivity, and molar volume. The inverse sum indeg index was found to be effective for molar refractivity, and the second modified Zagreb index was surface tension in linear regression models. In addition, the redefined third Zagreb index was the best predictor for polarizability and molar refractivity, while the second modified Zagreb index was effective for molar volume. The SDD index was found to be effective for surface tension in quadratic regression models.     

Determination of Uranium and Plutonium in High Active Solutions by Extractive Spectrophotometry

Plutonium and uranium was extracted from nitric acid into trioctyl phosphine oxide in xylene. The TOPO layer was analysed by spectrophotometry. Thoron was used as the chromogenic agent for plutonium. Pyridyl azoresorcinol was used as chromogenic agent for uranium. The molar absorption coefficient for uranium and plutonium was found to be 19000 and 19264 liter/mole-cm, respectively. The correlation coefficient for plutonium and uranium was found to be 0.9994. The relative standard deviation for the determination of plutonium and uranium was found to be 0.96% and 1.4%, respectively.     

Preparation of a cellulose-based enzyme membrane using ionic liquid to lengthen the duration of enzyme stability

A novel method for preparing enzyme membranes was developed. The enzyme was attached onto the electrode surface by dropping the enzyme solution and allowing it to dry. Glucose oxidase was used for entrapment. Then, the electrode surface was coated with an ionic liquid containing cellulose, and the ionic liquid was removed by immersing the electrode into water. Enzyme activity was retained in the membrane; the enzyme electrode can be used for detecting glucose in the range of 10 μM to 1 mM, and the response time was ~10 s. The stability duration of the electrode was examined: the enzyme electrode could be used for glucose detection for 6 months. The membrane was observed by atomic force microscopy in the force modulation mode; crystalline and amorphous parts were intermingled. In conclusion, the cellulose membrane can be a suitable immobilization matrix for enzymes.     

顶空气相色谱法测定输液器中环己酮残留

建立顶空气相色谱法测定输液器中环己酮残留量的分析方法。利用蠕动泵,以水为浸提介质,对输液器中的环己酮进行提取,采用顶空气相色谱法测定。色谱柱为Elite–5柱(30 m×0.32 mm,0.25μm),程序升温,初始温度为50℃保持3 min,以10℃/min升温至100℃,保持2 min,以20℃/min升温至170℃,保持2 min。FID检测器,检测器温度为250℃,进样口温度为230℃,分流比为5∶1,流量为2 m L/min,采用顶空进样。环己酮在0.494~98.700μg/m L范围内线性关系良好,相关系数r=0.999 9,方法定量限(S/N=10)为0.313μg/m L,测定结果的相对标准偏差小于1.0%(n=6),24 h模拟输液样品平均回收率为98.9%,循环浸提样品平均加标回收率为99.4%。该方法简单、快速、准确,可用于一次性使用输液器中环己酮残留量的检测。     

毛细管气相色谱法测定南美白对虾中硫丹的残留量

建立了运用毛细管气相色谱检测南美白对虾中硫丹残留的快速测定方法。用乙酸乙酯提取样品中的硫丹,提取液浓缩后以中性氧化铝和活性炭小柱进行双级柱色谱净化,用正己烷-乙酸乙酯(体积比为1∶1)洗脱,洗脱液用气相色谱-电子捕获检测器检测,以保留时间定性,外标法定量。在南美白对虾样品中分别添加0.20,0.10,0.04和0.02 mg/kg硫丹标准品,测得添加回收率为80.5%～109.5%,相对标准偏差为3.6%～8.4%。该方法在不具备凝胶渗透色谱条件下也能进行硫丹残留的检测,具有简便、准确的特点,能满足常规检测及食品安全监控的需要。     

Microdetermination of carbon and hydrogen in organic compounds using flushed-oxygen combustion tube

A rapid method of microanalysis for carbon and hydrogen in organic compounds using an empty combustion tube fused with two nozzles for flushing oxygen and employing reduced copper for the reduction of nitrogen oxide was investigated. A sample was decomposed rapidly in a sample heater for 2 min, and the gasified vapor was transported to the stationary combustion zone heated at 850 °C, where oxygen was flushing from two nozzles, the oxygen flow was then replaced with nitrogen for 3 min until all the combustion products were swept out towards the absorption train. The sample size was suggested to be around 1 mg for this rapid method, using a Mettler UM6, or an electrobalance having equal precision for the sampling.     

Analysis of glass by UV laser ablation inductively coupled plasma atomic emission spectrometry. Part 1. Effects of the laser parameters on the amount of ablated material and the temporal behaviour of the signal for different types of laser

Two lasers working in the UV part of the spectrum have been used for the analysis of glass samples. An XeCl excimer laser (308 nm) and a Nd:YAG laser operating at the third harmonic (355 nm) and the fourth harmonic (266 nm) have been selected. The energy was 100 mJ and 5 mJ for the excimer laser and the Nd:YAG laser, respectively. Because of different spot sizes, the fluence was of the same magnitude for both lasers. Crater characterization indicated that the laser ablation efficiency was similar for the two lasers when normalized to the same energy. However, the XeCl was found to be more efficient when the results were normalized to irradiance unit. The amount of probed material and ablated material was measured, leading to an efficiency higher than 80%. The influence of the glass colour and the laser wavelength was evaluated. The XeCl laser provided the largest amount of material but was sensitive to the glass colour. This laser was mainly suitable for bulk analysis. In contrast, the Nd:YAG, particularly at 266 nm, was insensitive to the glass colour and was appropriate for localized analysis. Inductively coupled plasma atomic emission spectrometry was used for atomization and excitation of the ablated material. A good agreement was found between the temporal behaviour of the amount of ablated material and the analyte signal.     

纳米固相微萃取应用于干红辣椒、水果饮料及红酒中罗丹明B的定量分析

制备了一种新型的聚苯乙烯纳米纤维, 将其作为固相萃取吸附剂装填制成固相萃取柱, 与高效液相色谱联用建立了干辣椒、 水果饮料及红酒中罗丹明B的定量分析方法. 高效液相色谱以3 g/L磷酸缓冲液-甲醇混合溶液(体积比3∶7, pH=7.0)为流动相. 通过对提取条件的优化, 得到该方法对干辣椒中罗丹明B的检出限为0.1 ng/g, 最低定量限为0.6 ng/g; 对水果饮料和红酒中罗丹明B的检出限均为0.2 ng/mL, 最低定量限均为0.5 ng/mL. 此方法对干辣椒中罗丹明B的提取回收率为98.2%~110.3%; 对水果饮料中罗丹明B的提取回收率为94.6%~102.2%; 对红酒中罗丹明B的提取回收率为90.4%~104.6%. 该方法的线性范围为1~100 ng/mL(ng/g), 相对标准偏差为2.3%~9.0%. 该方法灵敏度高、 选择性好, 可用于干辣椒、 水果饮料及红酒中罗丹明B的定量分析.     

Determination of Kynurenine and Tryptophan in Human Plasma by Stacking-Micellar Electrokinetic Chromatography

Kynurenine and tryptophan are important biomarkers for disorders in nervous and immune systems, while the low content of kynurenine in human plasma makes the determination by routine approaches difficult. In this work, an on-line preconcentration method for capillary electrophoresis was developed for the quantification of kynurenine and tryptophan. A concomitant sweeping phenomenon was observed due to the combination of micellar electrokinetic chromatography and stacking. The poor sensitivity in capillary electrophoresis was improved so that the determination of low concentrations of kynurenine became possible. Parameters that may affect the efficiency of the on-line concentration were systematically investigated and optimized. A large volume sample injection was employed for sampling at 100 mbar for 112 sec. A voltage of ?20 kV was applied, and the ionic sample matrix was removed with stacking while analytes were kept in the capillary. The voltage was switched to +18 kV and micellar electrokinetic chromatography was performed for separation and determination of kynurenine and tryptophan. Based on peak heights, the concentration factors for kynurenine and tryptophan were 33 and 31, respectively. The analytical performance of the established method was studied; good linearity of kynurenine was observed in the range of 0.3–30 µM (R² = 0.9988), and 0.3–60 µM (R² = 0.9963) was obtained for tryptophan. LODs of 0.15 µM for kynurenine and 0.30 µM for tryptophan were obtained. The optimum method was successfully tested in human plasma; kynurenine and tryptophan were well identified, which suggests that this method has potential for the analysis of biological samples.     

Determination of nebivolol and valsartan in a fixed-dose combination by liquid chromatography

An accurate and reproducible liquid chromatographic assay method was developed and validated for the determination of nebivolol and valsartan in a capsule formulation. Buffer-acetonitrile (55 + 45, v/v) was used for reversed-phase liquid chromatography to determine the contents of nebivolol and valsartan in the combination-capsule dosage form. The method was validated by determining parameters such as specificity, linearity, limits of detection and quantitation, precision, accuracy, and robustness. The method was found to be specific against placebo interference. Linearity was evaluated over the concentration ranges of 2-8 micro/mL for nebivolol and 32-128 microg/mL for valsartan (the correlation coefficient was 0.9999 for both nebivolol and valsartan). Both the intraday and interday precision values of the system and the method were determined. The accuracy of the method ranged from 100.66 to 102.58% for nebivolol and from 101.17 to 101.85% for valsartan. The proposed method was found to be robust when slight but deliberate changes were made in the analytical conditions. The developed method was found suitable for the assay determination of nebivolol and valsartan in a capsule formulation.     

Liquid chromatographic determination of simple phenolic compounds in waste waters from olive oil production plants.

A method was developed for the determination of simple phenolic compounds (PCs) in waste waters from olive oil production plants by liquid chromatography (LC). The sample under examination was acidified to pH 2 to precipitate proteins, acetone was added to eliminate the colloidal fraction, and hexane was used for extraction to eliminate lipidic substances. The solution obtained was filtered and injected into the LC system; the wavelength selected for the spectrophotometric detection was specific for PCs, so that carbohydrates, organic acids, and short-chain free fatty acids did not interfere. Recoveries of 9 PCs spiked to a real sample were 90-100% for concentrations ranging from 20 to 2000 mg/L for each analyte.     

Liquid chromatographic separation of derivatives of diospyrin, a bioactive bisnaphthoquinonoid plant-product, and analogous naphthyl compounds

Isocratic reversed-phase liquid chromatography (LC) method was developed using acetonitrile and water for the determination of diospyrin, a pharmacologically important bisnaphthoquinonoid plant-product. The method was validated for precision, accuracy and reproducibility, and was found to be linear over the concentration range of 1-1000 microg/ml; the limits of detection and quantitation were 8 and 20 ng, respectively. The technique was used to determine the amount of diospyrin in plant extracts from four climatic regions in India. It was also applied for differentiation and separation of 27 naphthyl compounds. While a composition of 50:50 was preferable for dimeric compounds, the composition 40:60 was a better choice for the monomers. Also, the isomeric alpha- and beta-naphthols and their dimers could be distinguished by conversion into the respective methyl ethers.     

高效液相色谱法同时测定牛肉及其制品中敌草隆、绿麦隆的残留量

介绍了用高效液相色谱同时测定牛肉及其制品中脲类除草剂——敌草隆、绿麦隆残留量的方法。色谱柱为ＳｅｌｅｃｔｏｓｉｌＣ１８柱,流动相为甲醇－水（６０∶４０,Ｖ／Ｖ）,ＵＶ－２４５ｎｍ检测。最小检测量：敌草隆为０．４ｎｇ,绿麦隆为０．５ｎｇ。线性范围均为０．０５～１０ｍｇ／Ｌ。回收率：敌草隆为８７．３４％～８７．６４％,绿麦隆为８８．７８％～９１．９４％。     

Solid-phase extraction of 4(5)-methylimidazole (4MeI) and 2-acetyl-4(5)-(1,2,3,4-tetrahydroxybutyl)-imidazole (THI) from foods and beverages with subsequent liquid chromatographic-electrospray mass spectrometric quantification

A method for the simultaneous determination of 4(5)-methylimidazole (4MeI) and 2-acetyl-4(5)-(1,2,3,4-tetrahydroxybutyl)-imidazole (THI) was developed using SPE and HPLC/MS. Solid-phase extraction using SCX Disc cartridges was used for isolation of the analytes from liquid samples. The lower LOQwas 0.1 ng/mL for 4MeI and 0.2 ng/ mL for THI. The linearity of the calibration curves was satisfactory as indicated by correlation coefficients >0.999. The CV for the intra- and inter-day precision was <5% (n = 6); the accuracy was in the range 98-103%. The recovery was > or = 97 and > or = 98% for THI and 4MeI, respectively. The method was used to determine THI and 4MeI in beverages, coffee, caramel colours and other samples.     

Feasibility of Separation and Quantification of Inorganic Arsenic Species Using Ion-Exchange Membranes and Laser-Induced Breakdown Spectroscopy

Analytical methods for the determination of inorganic arsenic species have attracted much attention due to the high toxicity of these compounds and related legislative regulations for food. A new method for the separation and quantitation of As(III) and As(V) was developed using ion-exchange membranes and laser-induced breakdown spectroscopy (LIBS). Using the anion-exchange polymer membrane, As(V) was selectively collected on the membrane, and As(III) was filtered through the membrane. The separated As(V) on the membrane was directly determined by LIBS. The As(III) in the filtrate was subsequently oxidized to As(V) and collected by the membrane for LIBS analysis. The detection limit for As(V) was estimated to be 10?mg/kg. The recovery efficiencies for the arsenic species as standards were in the range of 97–99%. This method was applied for the analysis As-spiked water certified reference materials, and the results showed that the recovery for As(V) was 98.9%. This new speciation method is cost-effective, simple, and low labor-intensive for the quantitation of inorganic arsenic.     

Determination of palladium and platinum by electrothermal atomic absorption spectrometry after deposition on a graphite tube

The inner wall of a pyrolytically coated graphite tube served as the surface for adsorptive accumulation and/or for electrodeposition of palladium and platinum. A flow system for this preconcentration was constructed. For the electrodeposition a three-electrode arrangement was used. The flow rate for deposition, the medium and deposition potentials were optimized. After the deposition step, the graphite tube was placed into the graphite furnace and an atomization programme was applied. The procedure was applied for the determination of Pd and Pt in airborne particulates.     

UV Index on tilted surfaces

Solar ultraviolet erythemal irradiance (UVER) has been studied on inclined planes with different orientations in Valencia, Spain. To do this a platform was designed that could turn through 90 degrees on its own axis. The radiometers were inclined at an angle close to the latitude of Valencia (39.5 degrees N). Using two timers the platform could be turned through 90 degrees every 5 min. On clear or partially cloudy days, including those with different turbidity values, it was observed that the UVER showed a maximum at 1200 h GMT, very close to solar noon, in the north and south positions, while the maximum for east and west orientations was found at approximately one hour before and one hour after midday respectively. It was also observed how the irradiance for the south orientation was greater and for the north was less than for the horizontal plane, as well as the opposite performances of the east and west orientations, for four days close to the summer and winter solstices and each equinox. Some experimental results were also compared with the results from the SMARTS2.9 model for the same conditions. It was found that the model frequently overestimated the experimental data. With respect to the maximum calculated UV Index in the different planes this was always higher for the south orientation than for the north, while it was similar for east and west orientations throughout the year. Finally the accumulated erythemal dosage for the considered period was obtained as a function of phototype and orientation, confirming that the accumulated erythemal dosage decreased by around 37% in the north orientation compared to the horizontal value, while in the south position it was only 6% less and some 20% and 15% less in the east and west positions, respectively.     

Determination of acyclovir in horse plasma and body fluids by high-performance liquid chromatography combined with fluorescence detection and heated electrospray ionization tandem mass spectrometry

Two methods are presented for the determination of 'respectively' the plasma protein unbound and total concentration of acyclovir in horse plasma and body fluids: first, a liquid-liquid extraction was performed on plasma, combined with HPLC-fluorescence detection for the total plasma concentration; second a more sensitive method using high-performance liquid chromatography combined with heated electrospray ionization tandem mass spectrometry (LC-HESI-MS/MS) was described for plasma and for body fluids analysis. To obtain the unbound concentration of acyclovir in plasma, a simple deproteinization step using a Microcon filter was performed. Ganciclovir was used as an internal standard. Analysis was carried out on an Inertsil 5 ODS-3 column for the HPLC-fluorescence method. For the LC-HESI-MS/MS method a PLRP-S column was used. The limit of quantification (LOQ) for the total concentration was set at 50 and 2 ng mL(-1) for the HPLC-fluorescence method and the LC-HESI-MS/MS method, respectively. The limit of quantification for the unbound concentration was set at 5 ng mL(-1) and at 2 ng mL(-1) for body fluids. The methods were successfully used to perform pharmacokinetic and clinical studies in horses after intravenous and oral dosage of acyclovir and its prodrug valacyclovir.     

Determination of oxycodone hydrochloride in oral solutions by high-performance thin-layer chromatography/densitometry

A thin-layer chromatography/densitometry method was developed and validated for the determination of oxycodone hydrochloride in oral solutions by using silica gel plates. A horizontal technique was used for development of the plates. The optimum composition for the mobile phase, which provided a suitable Rf value of 0.6 for oxycodone, was propanol-acetic acid-water-25% ammonia-methanol (20 + 1 + 1 + 3 + 10). Detection was at 234 nm. Oxycodone hydrochloride was stable on the sorbent and was precisely and accurately measured in the range of 0.3-1.5 microg/band.     

Densitometric Determination of Hecogenin from Agave americana Leaf Using HPTLC

We report a simple TLC densitometric method for the quantification of hecogenin from the leaves of Agave americana using HPTLC. The method was validated for precision, repeatability and accuracy. The method was found to be precise with RSD of 0.78 (intraday) and 0.82 (interday) for different concentrations of hecogenin. Instrumental precision was 0.42 (% RSD) for hecogenin. The content of hecogenin in different samples was estimated by the proposed method and was found to be in the range of 0.05−0.14% w/w in the samples analysed. Accuracy of the method was checked by conducting recovery study at three different levels for hecogenin and the average percentage recovery was 98.98%, 101.92% and 103.33%, respectively. The TLC densitometric method developed for the quantification of hecogenin was found to be simple, precise, specific, sensitive, accurate and can be used in routine quality control. Revised: 7 and 25 April 2006