TLC determination of mebendazol and pentoxifylline as residues on pharmaceutical equipment surfaces

This paper presents the applicability of thin-layer chromatographic methods with a subsequent densitometric or video densitometric quantitation for determination of residues in controlling pharmaceutical equipment cleanliness. Analytical methods were developed for monitoring residues of pentoxifylline at 10 mg/M2 and mebendazol at 1 mg/M2 on stainless steel surfaces. Simulated samples were prepared by addition of a calculated amount of pharmaceutical (as a solution) on a 35 x 35 cm stainless steel surface. After evaporation of solvent, the residues were wiped with wetted cotton. The cotton was extracted with dichloromethan-methanol (1 + 1). Filtered extract was concentrated by vacuum evaporation and an aliquot applied to the plate, where standards were also applied. In the narrow concentration range near the acceptable residue limits, linear calibration curve could be obtained for both substances. The mean recovery (n = 4) obtained by densitometric quantitation was 93.4% for pentoxifylline and 85.6% for mebendazol, with coefficients of variation of 3.5 and 8.3%, respectively. Results of video densitometric quantitation did not differ significantly. However, data acquisition and evaluation is faster compared with densitometry and allows better archiving possibilities as required by the regulatory authorities. Both quantitation modes can be applied to routine control of pharmaceutical equipment cleanliness.     

Fully automated open access platform for rapid, combined serial evaporation and sample reformatting

This paper reports a novel evaporator and its integration with an automated sample handling system to create a high throughput evaporation platform. The Vaportec V-10 evaporator uses a high speed rotation motor ( approximately 6000 rpm) to spin the vial containing a sample, creating a thin film of solvent which can be readily evaporated by the application of heat to the vial, while the consequent centrifugal force prevents "bumping". An intelligent algorithm controls pressure and temperature for optimum solvent removal conditions and end of run detection, critical for automation. The system allows the option of evaporation directly from a sample source vial, or alternatively, integrated liquid handling facilities provide the capability of transferring samples portionwise from a (large) source vial or bottle to a (small) daughter container, enabling efficient sample reformatting, with minimum user intervention. The open access system makes significant advances over current vacuum centrifugal evaporators in terms of evaporation rate and ease of automation. The evaporator's main features, the integration of robotics to provide automation, and examples of evaporation rates of a wide range of solvents from a variety of containers are described.     

Evaporation of substances under kinetic or diffusion control in sublimation in a vacuum

A diffusion-kinetic model of sublimation of substances in a vacuum is presented. The model defines two regions of the evaporation process depending on temperature: evaporation in the kinetic and diffusion control. The model was verified in experiments with benzoic acid and naphthalene by calculation of the sublimation rate of Zn, Co, V, and W, and by the known values of α.     

Simulation of photon intensity distributions to facilitate the design of beamlines at accelerator-based IR/THz sources

Simulations with the software Synchrotron Radiation Workshop (SRW) for the ANKA infrared (IR) beamlines IR1 and IR2 have shown, that the far-IR and terahertz (THz) edge radiation can interact with the vacuum chamber walls very close to the electron beam. Unfortunately SRW cannot compute wavefronts at large angles of observation and at a close vicinity to the source. As we need to take into account these perturbations for the further propagation of the radiation through the entire beamline optics to the experimental station, we have started to develop our own code.This code can generate the electric and magnetic field vectors by solving Maxwell equations without approximations and without restrictions to the angles of observation or distance to the source. In particular the latter requires that also the magnetic field vectors have to be calculated, to obtain the corresponding photon intensity distribution for situations where the electron beam intersects the observation plane.Moreover it revealed that it is essential to correct for the Coulomb field prior to calculating the photon intensity in cases where the electron beam intersects the observation plane. Therefore our code is not limited to synchrotrons but can also be used for the development of new kinds of IR/THz radiation facilities.     

Electrical and optical properties of C46H22N8O4KM (M=Co, Fe, Pb) molecular-material thin films prepared by the vacuum thermal evaporation technique

In this work, the synthesis of new materials formed from metallic phthalocyanines (Pcs) and double potassium salt from 1,8-dihydroxianthraquinone is reported. The newly synthesized materials were characterized by scanning electron microscope (SEM), atomic force microscopy (AFM), infrared (IR) and Ultraviolet-visible (UV-vis) spectroscopy. The powder and thin-film samples of the synthesized materials, deposited by vacuum thermal evaporation, show the same intra-molecular bonds as in the IR spectroscopy studies, which suggests that the thermal evaporation process does not alter these bonds. The effect of temperature on conductivity and electrical conduction mechanism was measured in the thin films (approximately 137 nm thickness). They showed a semiconductor-like behaviour with an optical activation energy arising from indirect transitions of 2.15, 2.13 and 3.6eV for the C(46)H(22)N(8)O(4)KFe, C(46)H(22)N(8)O(4)KPb and C(46)H(22)N(8)O(4)KCo thin films.     

顺酐生产中废水治理方法的改进

目前普遍应用的两种顺酐废水治理方法,生物法和传统真空蒸发法,都存在着运行成本高和不能将废水中有用物质充分回收的缺点.经过对传统真空蒸发法的改进和完善,使顺酐废水的治理既达到零排放的目的,又回收生产了富马酸合格产品,创造了经济效益.     

Rapid affinity purification of erythropoietin from biological samples using disposable monoliths

Identification of post-translational modifications of proteins in biological samples often requires access to preanalytical purification and concentration methods. In the purification step high or low molecular weight substances can be removed by size exclusion filters, and high abundant proteins can be removed, or low abundant proteins can be enriched, by specific capturing tools. In this paper is described the experience and results obtained with a recently emerged and easy-to-use affinity purification kit for enrichment of the low amounts of EPO found in urine and plasma specimens. The kit can be used as a pre-step in the EPO doping control procedure, as an alternative to the commonly used ultrafiltration, for detecting aberrantly glycosylated isoforms. The commercially available affinity purification kit contains small disposable anti-EPO monolith columns (6 μL volume, Ø7 mm, length 0.15 mm) together with all required buffers. A 24-channel vacuum manifold was used for simultaneous processing of samples. The column concentrated EPO from 20 mL urine down to 55 μL eluate with a concentration factor of 240 times, while roughly 99.7% of non-relevant urine proteins were removed. The recoveries of Neorecormon (epoetin beta), and the EPO analogues Aranesp and Mircera applied to buffer were high, 76%, 67% and 57%, respectively. The recovery of endogenous EPO from human urine was 65%. High recoveries were also obtained when purifying human, mouse and equine EPO from serum, and human EPO from cerebrospinal fluid. Evaluation with the accredited EPO doping control method based on isoelectric focusing (IEF) showed that the affinity purification procedure did not change the isoform distribution for rhEPO, Aranesp, Mircera or endogenous EPO. The kit should be particularly useful for applications in which it is essential to avoid carry-over effects, a problem commonly encountered with conventional particle-based affinity columns. The encouraging results with EPO propose that similar affinity monoliths, with the appropriate antibodies, should constitute useful tools for general applications in sample preparation, not only for doping control of EPO and other hormones such as growth hormone and insulin but also for the study of post-translational modifications of other low abundance proteins in biological and clinical research, and for sample preparation prior to in vitro diagnostics.     

Infrared controlled waxes for liquid handling and storage on a CD-microfluidic platform

A novel active valving technique, whereby paraffin wax plugs in microchannels on a centrifugal microfluidic platform are actuated using focused infrared (IR) radiation is demonstrated in this report. Microchannels were simultaneously or sequentially opened using a stationary IR source by forming wax plugs with similar or differing melting points. The presented wax plugs offer key advantages over current active valving techniques, including a less involved fabrication procedure, a simpler actuation process, and the ability to multiplex experiment with active valves. In addition, a new technique for automated liquid reagent storage and release on the microfluidic disc platform, based on the formation and removal of a wax layer, is demonstrated. Overall, the techniques presented in this report offer novel methods for liquid handling, separation, and storage on the centrifugal microfluidic disc platform.     

Perspectives in the development of the theory of spark-source and laser-plasma source mass-spectrometry

The processes of substance evaporation and atom ionization under different conditions of spark discharge or laser radiation are considered. It is shown that the dependence of the relative sensitivity coefficients on the properties of an element can be presented as the product of two exponents with parameters proportional to the atomization energies and first ionization potentials of the element. Differences in matrix composition and conditions influencing a sample in the ion source are considered by means of introducing two fitting parameters-atomization and ionization "temperatures"-into these exponents. Experiments carried out with the help of mass-spectrometers with spark and laser ion sources have corroborated the validity of the suggested quasi-equilibrium model and shown the possibility of its application for the improvement of the accuracy of analysis without use of standards as well as for checking the stability of experimental conditions in the process of analysis with standard samples.     

Use of an internal control for matrix-assisted laser desorption/ionization time-of-flight mass spectrometry analysis of bacteria

A method to aid in the analysis of bacterial samples of unknown concentration by matrix-assisted laser desorption/ionization (MALDI) mass spectrometry is demonstrated. It is shown that in MALDI analysis of bacteria, the intensities of resulting peaks in spectra are sensitive to the microbial concentration. At the high and low ends of the concentration range, no signal can be obtained, leaving very concentrated or very dilute samples indistinguishable. The addition of cytochrome c as an internal control allows the differentiation of these concentrated and dilute samples. The presence of the internal control causes only a 20% to 30% decrease in signal intensity when the bacterial concentration is optimum. However, the signal quality is improved when the internal control is added to some low concentrations of bacteria.     

Bead-based microfluidic toxin sensor integrating evaporative signal amplification

We have devised a microfluidic platform that incorporates substrate-laden silica beads for sensing the proteolytic activity of botulinum neurotoxin type A (BoNT/A)-one of the most poisonous substances known and a significant biological threat. The sensor relies on toxin-mediated cleavage of a fluorophore-tagged peptide substrate specific for only BoNT/A. Peptide immobilized on beads is recognized and cleaved by the toxin, releasing fluorescent fragments into solution that can be concentrated at an isolated port via evaporation and detected using microscopy. Evaporative concentration in combination with a specific channel geometry provides up to a 3-fold signal amplification in 35 min, allowing for detection of low levels of fluorophore-labeled peptide-a task not easily accomplished using traditional channel designs. Our bead-based microfluidic platform can sense BoNT/A down to 10 pg of toxin per mL buffer solution in 3.5 h and can be adapted to sensing other toxins that operate via enzymatic cleavage of a known substrate.     

Electrical and optical properties of copper and nickel molecular materials with tetrabenzo [b,f,j,n] [1,5,9,13] tetraazacyclohexadecine thin films grown by the vacuum thermal evaporation technique

Semiconducting molecular-material thin-films of tetrabenzo (b,f,j,n) {1,5,9,13} tetraazacyclohexadecine copper(II) and nickel(II) bisanthraflavates have been prepared by using vacuum thermal evaporation on Corning glass substrates and crystalline silicon wafers. The films thus obtained were characterized by infrared spectroscopy (FTIR), atomic force microscopy (AFM), ultraviolet–visible (UV–vis) spectroscopy and ellipsometry. IR spectroscopy showed that the molecular-material thin-films exhibit the same intra-molecular bonds as the original compounds, which suggests that the thermal evaporation process does not significantly alter their bonds. The optical band-gap values calculated from the absorption coefficient may be related to non-direct electronic interband transitions. The effect of temperature on conductivity was also measured in these samples. It was found that the temperature-dependent electric current is always higher for the nickel-based material and suggests a semiconductor-like behavior with conductivities in the order of 10^?8 Ω^?1 cm^?1.     

The evaporation characteristics of LiCl–KCl eutectic salt from uranium deposits using batch type vacuum distiller with temperature slope of each zones

Recovered salt can be reused in the electrorefining process and the final removed salt from uranium (U) deposits can be fed into a following U casting process to prepare ingot. Therefore, salt distillation process is very important to increase the throughput of the salt separation system due to the high U content of spent nuclear fuel and high salt fraction of U dendrites. Yields on salt recovered by a batch type vacuum distiller transfer device were processed for obtaining pure eutectic salt and U. In this study, the influence of the various temperature slopes of each zones on salt evaporation and recovery rate are discussed. From the experimental results, the optimal temperature of each zones appear at the Top Zone and Zone 1 is 850?°C, Zone 2 is 650?°C and Zone 3 is 600?°C, respectively. In these conditions, the complete evaporation of pure salt in 1.4?h occurred and the amount of recovered salt was about 99?wt%. The adhered salt in U deposits was separated by a temperature slope zone of salt distillation equipment. From the experimental results using U deposits, the amount of salt evaporation was achieved more than 99?wt% and the salt evaporation rate was about 1.16?g/min. Also, the mount of recovered salt was about 99.5?wt%.     

环境样品酞酸酯测定中降低空白值方法的探讨

针对环境样品酞酸酯分析中易受污染干扰的各个环节如玻璃器皿、溶剂空白、无水硫酸钠空白、仪器空白、全程空白等,做了仔细的空白值检查。结果表明,经铬酸洗液清洗过的玻璃器皿、试剂选用色谱纯或重蒸分析纯、无水硫酸钠临用前高温烘干、浓缩选用水浴自然蒸发或高纯氮气等措施均可大大降低背景空白值的干扰。并提出了降低空白值干扰的控制措施,以降低测定过程中的污染风险,保证测定结果的准确性和可靠性。     

The determination of bromide in natural waters by flow injection analysis

Bromide can occur in well waters as a result of sea water intrusion. The phenol red method is adapted to a flow-injection system and interferences are studied by using a two-channel valve. Standards are injected from one loop of the valve while the possible interferent is injected from the other loop; this provides a fast means of evaluating interferences. Ammonia, cyanide and humic substances interfere. Bromide can be determined down to 2 μM at a rate of 80 samples per hour     

A fully automated mass spectrometer for the analysis of organic solids

Automation of a mass spectrometer—computer system makes it possible to process up to 30 samples without attention after sample loading. An automatic sample changer introduces the samples successively into the ion source by means of a direct inlet probe. A process control unit determines the operation sequence. Computer programs are available for the hardware support, system supervision and evaluation of the spectrometer signals. The most essential precondition for automation — automatic evaporation of the sample material by electronic control of the total ion current — is confirmed to be satisfactory. The system operates routinely overnight in an industrial laboratory, so that day work can be devoted to difficult analytical problems. The cost of routine analyses is halved.     

Thin film deposition by means of laser ablation of titanium oxide targets in oxygen radiofrequency electrode plasma

The growth of titanium oxide films by means of target evaporation with a high-intensity laser radiation was studied. The experiments were conducted in vacuum, an oxygen atmosphere, an oxygen radiofrequency (RF) discharge plasma, and the plasma afterglow. It was shown that the use of RF discharge and the substrate mounted on the powered electrode makes it possible to preclude the formation of particles with a size above a few micrometers in the films and to increase their oxygen content, refractive index, and transmission coefficient, as well as the deposition rate.     

Possibilities of Density Functional Theory in Standardless Quantitative Spectral Analysis

Density functional theory can be used in the quantitative analysis of substances by their IR spectra in cases when high precision is not necessary or certified reference samples are principally unavailable or are difficult to obtain. IR spectra of 30 complex organic molecules including different heteroatoms (Br, Cl, F, N, O) were calculated using the Gaussian98w program (6-31G) basis set. The calculated spectra were compared with experimental ones, and quantitative inverse spectral problems (calculation of concentrations) were solved for all of the molecules studied. It was shown that the found concentrations for the majority of the studied substances differ from their true concentrations by no more than 30%, which is acceptable, for example, for ecological monitoring.     

Mechanism of the Immobilization of Surfactants on Polymer Surfaces by Means of an Argon Plasma Treatment: Influence of UV Radiation

The mechanism of the immobilization of the surfactant sodium 10-undecenoate (C11(:)) on poly(ethylene) (PE) by means of an argon plasma treatment has been investigated. In particular, the influence of the vacuum ultraviolet (UV) radiation emitted by the argon plasma on the immobilization was studied. For this purpose, PE samples were coated with C11(:) (PE/C11(:) samples) and treated with an argon plasma under different conditions. PE/C11(:) samples were placed inside (glow) and outside (afterglow) the visible region of the plasma. Additionally, polymer samples that were placed in the glow of the plasma were covered with lithium fluoride or quartz crystals. These materials are transparent for electromagnetic radiation with a wavelength longer than 104 and 150 nm, respectively. Derivatization X-ray Photoelectron Spectroscopy was applied to characterize the modified polymer surfaces. It was demonstrated that vacuum UV radiation with a wavelength shorter than 150 nm made a predominant contribution to the process of immobilization. Under certain conditions it was possible to retain about 30% of the functional groups of the initially coated surfactant layer on PE. Furthermore, the UV radiation accounted for etching of PE and PE/C11(:) surfaces and initiated oxidation of the polymer surfaces.     

Simultaneous determination of l-thyroxine (l-T(4)), d-thyroxine (d-T(4)), and l-triiodothyronine (l-T(3)) using a sensors/sequential injection analysis system

Requirements of high purity and enantiopurity for the raw materials of active substances used for the pharmaceutical formulations involved utilization of high reliable analytical techniques for the analysis of the active compound. Sequential injection analysis system with electrochemical sensors as detectors proved to be a very good alternative for the chromatographic methods, as it is more reliable, not expensive, and faster. Drugs containing only l-thyroxine (l-T(4)) or both l-T(4) and l-triiodothyronine (l-T(3)) are formulated for the dysfunctions of thyroid. A sequential injection analysis system that can use two amperometric immunosensors (for the assay of l-T(3) and l-T(4)) and an amperometric biosensor (for the assay of d-thyroxine, d-T(4)) as detectors is proposed for the purity and enantiopurity tests of the raw materials used for the formulation of the drugs for thyroid. The system proved to be very reliable. The three compounds can be determined on-line in synthesis process control with a frequency of 20 samples per hour.