Determination of sulfa antibiotic residues in river and particulate matter by field-amplified sample injection-capillary zone electrophoresis

In the present research, field-amplified sample injection–CZE (FASI–CZE) coupled with a diode array detector was established to determine trace level sulfa antibiotic. Sulfathiazole, sulfadiazine, sulfamethazine, sulfadimethoxine, sulfamethoxazole, and sulfisoxazole were selected as analytes for the experiments. The background electrolyte solution consisted of 70.0 mmol/L borax and 60.0 mmol/L boric acid (including 10% methanol, pH 9.1). The plug was 2.5 mmol/L borax, which was injected into the capillary at a pressure of 0.5 psi for 5 s. Then the sample was injected into the capillary at an injection voltage of –10 kV for 20 s. The electrophoretic separation was carried out under a voltage of +19 kV. The capillary temperature was maintained at 20˚C throughout the analysis, and six sulfonamides were completely separated within 35 min. Compared with pressure injection-CZE, the sensitivity of FASI-CZE was increased by 6.25–10.0 times, and the LODs were reduced from 0.2–0.5 to 0.02–0.05 μg/mL. The method was applied to the determination of sulfonamides in river water and particulate matter samples. The recoveries were 78.59–106.59%. The intraday and interday precisions were 2.89–7.35% and 2.77–7.09%, respectively. This provides a simpler and faster method for the analysis of sulfa antibiotic residues in environmental samples.     

Performance of a CW pumped Nd:YVO4 amplifier with kHz pulses

Until recently, simple and reliable high repetition-rate laser sources with nanosecond pulses much shorter than from conventional A-O Q-switch lasers were not available. However over the past 2 years we have developed such lasers based on proprietary fast E-O switching technology, which allows designs delivering 1 ns pulses and subnanosecond jitter for good synchronisation. The technology provides pulses with multi-kW peak power and repetition-rates to >100 kHz.Most recently, the performance of these short pulse lasers has been developed further by implementing oscillator/amplifier (master oscillator and power amplifier, MOPA) technology which increases the output to >1 W average power. Here we report on a simple model that has been used to predict the performance of the CW pumped Nd:YVO₄ amplifier used in the MOPA laser. The model is based on the well-known expressions for the saturated gain applying to laser pulses, but more usually applied to pulse-excited amplifiers. The model is shown to allow a good interpretation of the amplifier behaviour for kHz pulses and to be a useful tool for predicting the performance of the MOPA laser.     

LD泵浦固体激光器基模振荡光的场分布噪音

通过调整泵浦光直径,使得LD端面泵浦固体激光器的振荡光工作于基模.在排除高阶横模的条件下,测量了由于热透镜的不稳定引起的光场场分布的噪音.实验发现,基模振荡光的高斯半径、光束指向角都在波动,而且光斑存在畸变波动.对一个未采取抑制措施的2W连续LD端面泵浦Nd:YAG固体激光器进行了测量.结果表明,在总功率不变的情况下,激光束峰值点附近的光强波动达到6.3%;激光的高斯半径波动达到5.8%;激光的指向角波动达到0.3mrad.     

低阻抗二极管产生的强流电子束能谱分布的数值模拟

 给出了低阻抗二极管产生的电子束能谱分布及外加磁场对二极管阻抗影响的数值模拟研究结果。结果表明，即使在外加电压恒定的条件下，二极管产生的电子束也具有一定的能谱分布，这说明用二极管电压、电流波形计算脉冲电子束能谱分布是不正确的。另外,外加磁场对低阻抗二极管的阻抗特性具有较大影响，其阻抗随外加磁场的增大而减小。分析认为这是由于外加磁场强度的变化改变了二极管中束电子的运动轨迹。当没有外加磁场或外加磁场较小时，低阻抗二极管产生的电子束发生自箍缩，此时二极管电流是自箍缩饱和顺位流；当外加磁场足够强时，电子束的自箍缩被抑制，二极管电流是没有箍缩时的空间电荷限制电流。束电流小于自箍缩临界电流的二极管其阻抗将不随外加磁场的变化而变化。     

消除预脉冲电压的撬棒管开关法

 分析了脉冲线加速器在放电过程中产生的预脉冲电压现象。为了减少预脉冲电压引起的等离子体发射对正常状态的影响，采用了一种冷阴极撬棒管，将它与阴极杆相连。实验证明在采用了这种器件后，预脉冲电压可以从150kV左右减少到50kV。相对论返波管和相对论磁控管的性能得以显著改善。     

Analysis of basic hair dyes by HPLC with on-line post-column photochemical derivatisation

Summary A reversed phase liquid chromatographic method is proposed for the analysis of basic hair dyes (raw materials and colourant formulations). The performance of the method was enhanced by introducing post-column on-line photochemical derivatisation in combination with a Diode Array Detector. On-line photoderivatisation provided an effective way of selectively transforming the analytes to compounds with different spectral properties. For each analyte two characteristic UV-Visible spectra (photoreactor on and off) were obtained with the same mobile phase and this information in combination with the chromatographic data (k' at pH 3.0 and 4.5) enabled the unambiguous identification of both commonly used, approved, and banned basic hair dyes. Additionally, this approach was found useful to improve the method sensitivity, allowing the determination of analytes present in low concentration (0.03%) in complex commercial formulations.This work constitutes part of the thesis for the Dottorato di Ricerche of Roberto Gotti.     

In situ sensing of the middle atmosphere with balloonborne near-infrared laser diodes

Since 1997, two near-infrared laser diode sensors have been developed with the support of the CNES, the French space agency, to provide in situ data of H(2)O, CH(4) and CO(2) in the middle atmosphere. The realized instruments were flown from stratospheric balloons within the framework of European campaigns for the study of stratospheric ozone and water vapor and were involved in the validation of the ODIN and ENVISAT satellites. In this paper, we describe the developed laser probing technique, we report atmospheric measurements and finally we discuss future perspectives, particularly the in situ laser sensing of the lower atmosphere of Mars and the implication of the laser hygrometers in balloon campaigns at mid-latitudes and tropical regions to investigate the sources and sinks of stratospheric H(2)O.     

An analysis of avidin, biotin and their interaction at attomole levels by voltammetric and chromatographic techniques

The electroanalytical determination of avidin in solution, in a carbon paste, and in a transgenic maize extract was performed in acidic medium at a carbon paste electrode (CPE). The oxidative voltammetric signal resulting from the presence of tyrosine and tryptophan in avidin was observed using square-wave voltammetry. The process could be used to determine avidin concentrations up to 3 fM (100 amol in 3 l drop) in solution, 700 fM (174 fmol in 250 l solution) in an avidin-modified electrode, and 174 nM in a maize seed extract. In the case of the avidin-modified CPE, several parameters were studied in order to optimize the measurements, such as electrode accumulation time, composition of the avidin-modified CPE, and the elution time of avidin. In addition, the avidin-modified electrode was used to detect biotin in solution (the detection limit was 7.6 pmol in a 6 l drop) and to detect biotin in a pharmaceutical drug after various solvent extraction procedures. Comparable studies for the detection of biotin were developed using HPLC with diode array detection (HPLC-DAD) and flow injection analysis with electrochemical detection, which allowed biotin to be detected at levels as low as 614 pM and 6.6 nM, respectively. The effects of applied potential, acetonitrile content, and flow rate of the mobile phase on the FIA-ED signal were also studied.     

Tests for liquid chromatographs

Summary The paper describes tests for liquid chromatographs to assess the autosampler and pump flow rate precision; suitability of the instrument for normal phase chromatography; UV detector performance; and external band broadening characteristics. Tests for mixing and proportioning characteristics of solvent pumps and performance of diode array detectors are also considered. These tests are designed to evaluate the performance of both newly released liquid chromatography equipment and equipment already in operation. Data from evaluations carried out by instrument manufacturer’s and suppliers is reported and discussed. This data offers specifications to a common format for initial selection of instruments prior to purchase.     

Application of diode array detectors for solute identification in toxicological analysis

Summary The possibilities and limitation of automated solute identification via UV/VIS spectroscopy in HPLC are demonstrated and applications in toxicologic analysis are described. A standard isocratic system is used. The influence of various chromatographic parameters on retention time is shown. A retention time window of ±15% is required. In addition to retention time, derived spectral data are calculated (minima and maxima of derivatives, area counts under standardized spectral ranges, absorption at various wavelength) and used for positive solute identification. It is possible to identify solutes with a high degree of certainty in urine and plasma if their concentration is at least 10 ppm.