HPLC of antibiotics. 1. Streptolydigin and related compounds

Two new acyltetramic acids related to streptolydigin have been isolated from fermentations of Streptomyces lydicus. The principal members of this complex were resolved by TLC on silica gel. However, the methods of detection, permanganate spray or bioautography, were not suitable for both crude fermentation broths and purified extracts. Gas chromatography is unsuitable for the detection of either underivatized or silylated streptolydigins. High performance liquid chromatography (HPLC) particularly on triethylaminoethyl cellulose is rapid and sensitive and is the method of choice for the analysis of both crude and purified samples. Using high performance liquid chromatography, two components were detected in the complex, which are not observed using any of the other chromatographic procedures.     

Determination of acidic chlorinated pesticides in water: Comparison of official EPA method 515.1 and liquid-solid extraction HPLC/UV and HPLC/PBMS analyses

Summary A comparison of the official EPA method 515.1 for determination of chlorinated acidic pesticides and a modification of it is illustrated. Extraction of the analytes from water and their determination and quantitation is by gas chromatography-electron capture detection (GC-ECD), liquid chromatography-UV detection and liquid chromatography-particle beam mass spectrometry. Although HPLC-PBMS was found to be less sensitive than the GC-ECD method, it was, nevertheless, more sensitive than HPLC-UV. The modified method is simpler, quicker and allows more accurate determination of pesticides in aqueous samples.Deceased July 31, 1996     

A method for correcting the contact angle from the θ/2 method

The θ/2 method, a widely used technique on measuring the contact angle of a sessile drop, assumes that the drop profile is part of a sphere. However, the shape profile of a sessile drop is governed by the Young–Laplace equation and is different from a sphere, especially for drops with a large bound number (e.g. large volume or small surface tension). The spherical assumption, therefore, causes errors on evaluating the contact angles. The deviation of contact angle from the θ/2 method is evaluated from a theoretical calculation in this work. A simple means is given for correcting the measurement error. The corrected angle results from the drop volume, surface tension, liquid density and the contact angle from θ/2 method. An algorithm for finding the correct contact angle without knowing the density and surface tension is also given. At the end, two examples of pendant drops are given for the illustration.     

STRUCTURE EVOLUTION OF POLYMER CHAINS FOR NECKING FORMATION IN HIGH-SPEED FIBER SPINNING PROCESS

Finite element method is used to simulate the high-speed melt spinning process,based on the equation system proposed by Doufas et al.Calculation predicts a neck-like deformation,as well as the related profiles of velocity,diameter, temperature,chain orientation,and crystallinity in the fiber spinning process.Considering combined effects on the process such as flow-induced crystallization,viscoelasticity,filament cooling,air drag,inertia,surface tension and gravity,the simulated material flow behaviors are consistent with those observed for semi-crystalline polymers under various spinning conditions.The structure change of polymer coils in the necking region described by the evolution of conformation tensor is also investigated.Based on the relaxation mechanism of macromolecules in flow field different types of morphology change of polymer chains before and in the neck are proposed,giving a complete prospect of structure evolution and crystallization of semi-crystalline polymer in the high speed fiber spinning process.     

Validation of a screening method for the simultaneous identification of fat-soluble and water-soluble vitamins (A,E, B<Subscript>1</Subscript>, B<Subscript>2</Subscript> and B<Subscript>6</Subscript>) in an aqueous micellar medium of hexadecyltrimethylammonium chloride

Simultaneous determination of the fat-soluble vitamins A and E and the water-soluble vitamins B₁, B₂ and B₆ has been carried using a screening method from fluorescence contour graphs. These graphs show different colour zones in relation to the fluorescence intensity measured for the pair of excitation/emission wavelengths. The identification of the corresponding excitation/emission wavelength zones allows the detection of different vitamins in an aqueous medium regardless of the fat or water solubility of each vitamin, owing to the presence of a surfactant which forms micelles in water at the used concentration (over the critical micelle concentration). The micelles dissolve very water insoluble compounds, such as fat-soluble vitamins, inside the aggregates. This approach avoids the use of organic solvents in determining these vitamins and offers the possibility of analysing fat- and water-soluble vitamins simultaneously. The method has been validated in terms of detection limit, cut-off limit, sensitivity, number of false positives, number of false negatives and uncertainty range. The detection limit is about g L^–1. The screening method was applied to different samples such as pharmaceuticals, juices and isotonic drinks.     

微波－气相－热压法分解高纯铂的研究

本文研究了微波气相热压法新技术分解高纯铂在密闭的聚四氟乙烯高压罐中，以微波瞬间加热混合酸产生的高压、纯净蒸气分解金属铂，此法避免了酸中杂质的沾污以制备供高纯铂分析的试液，提高了痕量杂质分析的准确度和降低检测限     

对固体圆二色光谱测试方法的再认识——兼谈“浓度效应”

对近期发展的固体圆二色(CD)光谱测试方法进行了概述、评价和比较, 着重探讨了“浓度效应”的存在使固体CD光谱失真的原因. 通过对本课题组和其他作者已报道的四种化合物的固体CD谱再测试的反思, 强调了依手性化合物的手性光谱学性质不同, 根据浓度梯度实验选择其合适测试浓度的必要性. 对固有手性的阻转异构化合物(S)-1,1'-联二萘酚(S-BINOL)进行了成膜法固体CD谱浓度梯度测试, 发现所得固体薄膜CD谱中也存在着“浓度效应”     

Investigation of the limitations of saturated fractional factorial experimental designs,with confounding effects for an HPLC ruggedness test

Summary Recently much attention has been directed to the validation of analytical methods. The level of validation will depend on the method application. If a method is developed for general use, for instance by different analysts, instruments or laboratories, then the effect of these changes need evaluation. This is normally referred to as ruggedness testing, where the limitations of the method to changes in the specified conditions are examined.This paper examines the use of Plackett-Burman fractional factorial experiment designs for ruggedness testing in high performance liquid chromatography (HPLC). The ability of these designs to identify confounding effects is applied to the stability indicating analysis of Salbutamol and its major degradation product, AH4045. The results show that confounding effects, proving extremely pertinent to HPLC, can be identified.The assay proved rugged to most tested changes although not to the use of column packing material from different manufacturers.     

Nonlinear vertical accelerations of a floating torus in regular waves

The longitudinal motions and vertical accelerations of a floating torus as well as wave motion inside the torus are studied by model tests in regular deep-water waves. Comparisons are made with linear and partly with second-order potential-flow theory for the smallest examined experimental wave height-to-wave length ratio 1/120. Reasonable agreement is obtained, in particular for the linear problem. The importance of 3D flow, hydroelasticity and strong hydrodynamic frequency dependency is documented. Experimental precision errors and bias errors, for instance, due to tank-wall interference are discussed. Numerical errors due to viscous effects are found to be secondary. Experiments show that the third and fourth harmonic accelerations of the torus matter and cannot be explained by a perturbation method with the wave steepness as a small parameter.     

A generic framework for time-stepping partial differential equations (PDEs): general linear methods,object-oriented implementation and application to fluid problems

Time-stepping algorithms and their implementations are a critical component within the solution of time-dependent partial differential equations (PDEs). In this article, we present a generic framework – both in terms of algorithms and implementations – that allows an almost seamless switch between various explicit, implicit and implicit–explicit (IMEX) time-stepping methods. We put particular emphasis on how to incorporate time-dependent boundary conditions, an issue that goes beyond classical ODE theory but which plays an important role in the time-stepping of the PDEs arising in computational fluid dynamics. Our algorithm is based upon J.C. Butcher's unifying concept of general linear methods that we have extended to accommodate the family of IMEX schemes that are often used in engineering practice. In the article, we discuss design considerations and present an object-oriented implementation. Finally, we illustrate the use of the framework by applications to a model problem as well as to more complex fluid problems.