全自动在线固相萃取-液相色谱-高分辨质谱法测定麦卢卡蜂蜜中的特征标志物

建立了全自动在线固相萃取-液相色谱-高分辨质谱(SPE-LC-HRMS)测定麦卢卡蜂蜜中特征标志物3,5-二甲氧基苯甲酸甲酯-4-双葡萄糖糖苷(leptosperin)的方法。以Dikma Diamonsil Plus C_(18)色谱柱(150 mm×4.6 mm,5μm)为分析柱,0.1%(v/v)甲酸水溶液-乙腈为流动相进行梯度洗脱,在电喷雾负离子、目标二级离子扫描模式下进行检测,外标法定量。结果表明,在0.5~100.0 mg/L范围内该分析物的线性关系良好,相关系数为0.999 3,方法的检出限(LOD,S/N≥3)和定量限(LOQ,S/N≥10)分别为3 mg/kg和10 mg/kg。在不同蜂蜜样品中分别添加50.0、100.0、200.0 mg/kg(洋槐蜜中添加10.0、20.0、50.0 mg/kg)特征化合物标准品进行加标回收率试验,平均回收率为82.0%~95.2%,相对标准偏差为2.7%~9.7%(n=6)。利用该方法对来自新西兰12种不同品种的95个蜂巢成熟原蜜和来自4个国家50个商品化蜂蜜进行了验证。该法快速、灵敏、准确,可为解决进口新西兰麦卢卡蜂蜜的判别难题提供技术支持。     

Direct detection of nanoparticles and components in smoke by time-of-flight mass spectrometry with soft plasma ionization

A new system combining a soft plasma ionization (SPI) source with a time-of-flight mass spectrometer (TOFMS) has been successfully developed and applied to direct and on-line analysis of nanoparticles in smoke generated during combustion of mosquito coils with no sample preparation. The mass spectra of nanoparticles in smoke were examined in conjunction with the effects of species, pressure and current of the SPI discharge on fragmentation. The results indicated that a maximum mass of m/z 1576 was detectable when the following optima SPI conditions were satisfied: a He gas pressure of 1000 Pa with an air pressure of 1600 Pa and a discharge current of 110 mA. Furthermore, considering the results for emission spectra we suppose an ionization mechanism of SPI in which excitation and ionization of nitrogen molecule is promoted by the presence of He gas, leading to promote the smoke sample ionization. The mass spectrum of nanoparticles showed specific patterns of a peak interval of 74 which were assigned to triacetylene (1,3,5-hexatriyne). The most abundant peak in the mass spectrum, at m/z 452, was assigned to triacontanoic acid.     

Determination of Chloride Content in Different Types of Cement Using Laser-Induced Breakdown Spectroscopy

The characterization and accurate determination of the chloride content in cement/concrete is very important for the assessment of the durability and safety of a concrete structure. The available analytical techniques are relatively expensive and time consuming. In this study, a laser-induced breakdown spectroscopy (LIBS) system was used for determination of elemental composition in three different types of cement samples. The plasma was generated by focusing a pulsed Nd: YAG laser at 1064 nm on the cement samples. The concentrations of different elements of significance for structural stability in cement samples were determined. The evaluation of the potential and the capabilities of LIBS as a rapid tool for characterization of cement samples is discussed. The optimum LIBS setup and experimental conditions to detect and measure chloride in building materials are reported. The LIBS results were compared with the results obtained using a standard analytical technique such as inductively coupled plasma emission spectroscopy (ICP–ES). The limits of detection were determined, and calibration curves were measured. The results of this investigation indicate the reliability of LIBS to characterize different cement samples and to assess the chloride content in these cements.     

On-line detection of emulsion polymerization by solid-state NMR spectroscopy

 The on-line detection of emulsion polymerization processes by means of solid-state NMR spectroscopy is demonstrated for the first time using poly(butyl acrylate) as a model system. Relatively short time intervals are accessible via ¹H detection while the use of ¹³C NMR spectroscopy results in an increased spectral resolution. Details of sample preparation and experimental techniques are given, while remaining artifacts of the preliminary results will be addressed in further investigations. Received: 7 November 1997 Accepted: 5 January 1998     

Monitoring process for attributes with quality deterioration and diagnosis errors

The aim of this paper is to present an online economical quality-control procedure for attributes in a process subject to quality deterioration after random shift and misclassification errors during inspections. The process starts in control (State I) and, in a random time, it shifts to out of control (State II). Once at State II, the non-conforming fraction increases according to a non-decreasing function ψ(z), where z is the number of items produced after a shift. The monitoring procedure consists of inspecting a single item at every m produced items, which is examined r times independently to decide its condition. Once an inspected item is declared non-conforming, the process is stopped and adjusted. A direct search technique is used to find the optimum parameters which minimize the expected cost function. The proposed model is illustrated by a numerical example. Copyright © 2007 John Wiley & Sons, Ltd.     

微波炉在流动注射体系中的在线应用

微波炉在流动注射体系中的在线应用是近１０年来发展的一项新技术，在样品的在线分解和加速流动注射分析中指示反应速度方面获得广泛应用。本文从仪器技术、结果和应用几个方面概述了从１９８６年以来这项技术的发展。     

On-line small-angle and wide-angle x-ray scattering studies on melt-spinning poly(vinylidene fluoride) tape using synchrotron radiation

On-line small-angle and wide-angle x-ray scattering experiments were performed during the melt spinning of polyvinylidene fluoride using the DESY synchrotron light source. In these studies, the melt-spinning apparatus consisting of a screw extruder, a metering pump, and a take-up motor system were assembled on two separate stepper-motor-driven platforms. To investigate the structure development during crystallization, the tape location at the desired distance from the die could be positioned at the beam level with synchronous vertical movement of extruder and take-up platforms. Small-angle and wide-angle x-ray patterns were taken simultaneously with a two-dimensional wire detector and one-dimensional wire detector. In a separate study, two-dimensional WAXS data were also taken under identical processing conditions to observe the off-equator diffraction behavior during the crystallization. The data obtained for a variety of take-up speeds generally indicate that SAXS d-spacings first appear large in the early stages of crystallization and gradually decrease along the spin-line (as the crystallization progresses). As the take-up speed increases, the crystallization onset position moves away from the die and d-spacings observed at the onset increase. In addition, the shape of the discrete scattering pattern starts as a meridional streak and converts to a teardrop shape with the tip of the pattern pointing toward the beam stop at the early stages of crystallization for high take-up speeds. This does not occur at low take-up speeds and is attributed to the differences in crystallization behavior which is spherulitic or sheaflike to row nucleated crystallites. Our studies also showed that SAXS patterns appear earlier than the wide-angle crystalline diffraction peaks indicating the SAXS technique to be more sensitive to the structural changes at these stages. An idealized model is developed to explain the observed patterns at high take-up speeds. This consists of two regimes. In regime 1, the periodic fluctuations due to the alternating crystalline and amorphous regions form along the regions where eventually the “shish” structures develop. In the second stage, a volume filling crystallization takes place between the existing crystallites along the shish structure and simultaneously radial overgrowth of crystallites (i.e., the “kebabs”) takes place. This causes the observed reduction in the average d-spacing. © 1993 John Wiley & Sons, Inc.     

Highly sensitive differential pulse amperometric detection of second generation anti-tumor platinum compounds in HPLC effluents

Summary A highly sensitive on-line amperometric detection of platinum compounds in HPLC effluents was possible with the use of a polarographic detector. For TNO-1 (=cis-1,1-di(aminomethyl)-cyclohexane Pt(II)chloride) a linear dynamic range of at least three decades could be obtained (0.034–108g TNO-1/ml) with a detection limit of three times the noise signal at 0.7 ng TNO-1 (20ng Pt/ml). The sensitivity was 0.1 nA/ng TNO-1 (0.2nA/ng Pt). The within-day presicion was 1.1% at a concentration of 10.8g TNO-1/ml (n=10). With this system the compatibility was measured of TNO-6 with infusion fluids. In 0.15 M NaCl, TNO-6 (=cis-1,1-di(aminomethyl)-cyclohexanePt(II)sulphate) was converted into TNO-1 within 40 minutes. Molecular changes of TNO-6 were also observed in a 5% aqueous glucose solution.     

A Flexible On-line Scheduling Algorithm for Batch Machine with Infinite Capacity

We study on-line scheduling on a batch machine with infinite capacity. We present a flexible on-line scheduling algorithm that aims at minimizing the makespan and achieves the optimal competitive ratio of . This research is substantially supported by a grant from City University of Hong Kong (Grant No. 7001119). The second author is supported by this grant and by the Natural Science Foundation of China.     

Optical Measuring Method for Quality Monitoring Purpose in Laser Welding of Tin－plates

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