H+ISFET-based biosensor for determination of penicillin G

A biosensor based on an H+ ion sensitive field effect transistor (H+-ISFET) and penicillin G acylase has been developed. The response time of the sensor to different concentrations of penicillin G was 30 s. In a 20 mM phosphate buffer at pH 7.0, the linear range of the calibration curve was from 0.5 to 8 mM. The coefficients of variation for three samples with 20 repeated measurements were below 5%. Stability of the sensor could reach about 6 months and more than 1000 runs were performed without a significant decrease of the output value. The sensor was tested for measurement of the penicillin G content in penicillin fermentation broth. Forty samples with low and high concentrations of penicillin G were chosen for the correlation test. The values assayed by the sensor method were compared with the values assayed by HPLC method, the correlation coefficient (r) was 0.9944 and the regression equation was y = 1.034X - 2083.7 respectively. The different measuring methods are discussed in the text. (C) 1998 Published by Elsevier Science S.A. All rights reserved.

The design structure system - A method for managing the design of complex systems

Systems design involves the determination of interdependent variables. Thus the precedence ordering for the tasks of determining these variables involves circuits. Circuits require planning decisions abut how to iterate and where to use estimates. Conventional planning techniques, such as critical path, do not deal with these problems. Techniques are shown in this paper which acknowledge these circuits in the design of systems. These techniques can be used to develop an effective engineering plan, showing where estimates are to be used, how design iterations and reviews are handled, and how information flows during the design work.

Determination of AlxGa1-xAs Auger sensitivity factors

AlxGa1-xAs Auger sensitivity factors have been determined by using PHI610 scanning Auger microprobe with pure elemental standards Al, Ag and matrix GaAs. The quantitative results of AlxGa1-xAs measured by the present method are in very good agreement with X-ray double crystal measurements. it is shown that by using sensitivity factors obtained from the self-instrument, the accuracy of the quantitative AES analysis can be considerably improved compared with that using elemental relative sensitivity factors given by the PHI handbook or internal standard method.

Determination of the interdiffusion coefficients of liquid Zn and Sn using Ta/Zn-Sn/Si trilayers

In this paper we present a new method for measuring diffusion coefficients in liquid metals under convection-less conditions with solid/liquid-liquid/solid trilayer. The advantage of this kind of trilayer is that effects from gravity-induced convection and Marangoni-convection can be omitted, so that the diffusion coefficient is determined more accurately. The Ta/Zn-Sn/Si trilayer were prepared with a multi-target ion-beam sputtering deposition technique and annealed in an electric furnace under an argon atmosphere. The interdiffusion of liquid zinc and tin at 500 degrees degree C was investigated. The diffusion concentration profiles were determined by energy dispersive spectroscopy. The interdiffusion coefficients range from 1.0x10(-6)cm(2)/s to 2.8x10(-6)cm(2)/s, which is less than previous values measured by capillary reservoir technique under 1g-environment where various convection exist. The precise interdiffusion coefficients of liquid zinc and tin result from the removing of disturbances of various kinds of convection.

Determination and identification of isoflavonoids in Radix astragali by matrix solid-phase dispersion extraction and high-performance liquid chromatography with photodiode array and mass spectrometric detection

The isoflavonoids in Radix astragali were determined and identified by HPLC-photodiode array detection-MS after extraction employing matrix solid-phase dispersion (MSPD). As a new sample preparation method for R. astragali, the MSPD procedure was optimized, validated and compared with conventional methods including ultrasonic and Soxhlet extraction. The amounts of two major components in this herb, formononetin (6) and ononin (2), were determined based on their authentic standards. Four major isoflavonoids, formononetin (6), ononin (2), calycosin (5) and its glycoside (1), and three minor isoflavonoids, (6aR,11aR)-3-hydroxy-9, 10-dimethoxypterocarpan (7), its glycoside (3), and (3R)-7,2'-dihydroxy-3',4'-dimethoxyisoflavone-7-O-beta-D-glycoside (4), were identified based on their characteristic two-band UV spectra and [M + H](+), [aglycone + H](+) and [A1 + H](+) ions, etc. The combined MSPD and HPLC-DAD-MS method was suitable for quantitative and qualitative determination of the isoflavonoids in R. astragali. (C) 2003 Elsevier B.V. All rights reserved.

Determination of urinary oxidative DNA damage marker 8-hydroxy-2 '-deoxyguanosine and the association with cigarette smoking

8-hydroxy-2'-deoxyguanosine (8OHdG) has been widely used as a biomarker of oxidative DNA damage in both animal models and human studies. To evaluate the effect of cigarette smoking on oxidative stress, we studied the levels of urinary 8OHdG from smokers and non-smokers and investigated the association with cigarette smoking. The urinary 8OHdG concentrations were determinated by capillary electrophoresis with end-column amprometric detection (CE-AD) after a single-step solid phase extraction (SPE), and then quantitatively expressed as a function of creatinine excretion. To increase the concentration sensitivity, a dynamic pH junction was used and the focusing effect was obvious when using 30 mM phosphate (pH 6.50) as sample matrix. The limit of detection is 4.3 nM (signal-to-noise ratio S/N = 3). The relative standard deviation (R.S.D.) was 1.1% for peak current, and 2.3% for migration time. Based on the selected CE-AD method, it was found that the mean value of urinary 8OHdG levels in the smokers significantly higher than that in non-smokers (31.4 +/- 18.9 nM versus 14.4 +/- 7.6 nM, P = 0.0004; 23.5 +/- 21.3 mug g(-1) creatinine versus 12.6 +/- 13.2 mug g(-1) creatinine, P = 0.028). (C) 2004 Elsevier B.V. All rights reserved.

Determination of sulfur-containing compounds in diesel oils by comprehensive two-dimensional gas chromatography with a sulfur chemiluminescence detector

This article reports an analytical method for separating, identifying and quantitating sulfur-containing compounds and their groups in diesel oils (170-400degreesC) using comprehensive two-dimensional gas chromatography coupled with a sulfur chemiluminescence detector. The identification of target compounds and their groups was based on standard substances, the group separation feature and the-effect of comprehensive two-dimensional gas chromatography. The quantitative analysis on major sulfur compounds and total sulfur was carried out based on the linear response of sulfur chemiluminescence detector and the internal standards method. The results of total sulfur determination in the samples were compared with those from ASTM D 4294 standard method, the R.S.D. percentage were <6.02%, correctness of this method can meet the industrial requirement. To the end, the method developed was used to investigate the sulfur-containing compounds in different diesel oils, the result shows that the distribution of sulfur-containing compounds in diesel oils from different process units are apparently different. The sulfur compounds in fluid catalytic cracking (FCC), residuum fluid catalytic cracking (RFCC) diesel oils mainly exist in the form of alkyl-substituted dibenzothiophenes that add up to about 40-50% of the total sulfur, while this number is only 6-8 and 20-28% in visbreaking (VB) and delayed-coking (DC) diesel oils, respectively. (C) 2003 Elsevier B.V. All rights reserved.

The application of spline wavelet transform to the determination of electroosmotic mobility in capillary electrophoresis

The rule of current change was studied during capillary electrophoresis (CE) separation process while the conductivity of the sample solution was different from that of the buffer. Using a quadratic spline wavelet of compact support, the wavelet transforms (WTs) of capillary electrophoretic currents were performed. The time corresponding to the maximum of WT coefficients was chosen as the time of current inflection to calculate electroosmotic mobility. The proposed method was suitable for different CE modes, including capillary zone electrophoresis, nonaqueous CE and micellar electrokinctic chromatography. Compared with the neutral marker method, the relative errors of the developed method for the determination of electroosmotic mobility were all below 2.5%. (C) 2002 Elsevier Science B.V. All rights reserved.

Determination of peptides and amino acids from wool and beer with sensitive fluorescent reagent 2-(9-carbazole)-ethyl chloroformate by reverse phase high-performance liquid chromotography and liquid chromotography mass spectrometry

A new method for the sensitive determination of amino acids and peptides using the tagging reagent 2-(9-carbazole)-ethyl chloroformate (CEOC) with fluorescence (FL) detection has been developed. Identification of derivatives was carried out by liquid chromotography mass spectrometry. The chromophore in the 2-(9-fluorenyl)-ethyl chloroformate (FMOC) reagent was replaced by carbazole, which resulted in a sensitive fluorescence lerivatizing agent CEOC. CEOC can easily and quickly label peptides and amino acids. Derivatives are stable enough to be efficiently analyzed by high-performance liquid chromatography. Studies on derivatization demonstrate excellent derivative yields over the pH range 8.8-10.0. Maximal yields close to 100% are observed with three- to fourfold molar reagent excess. Derivatives exhibit strong fluorescence and allow direct injection of the reaction mixture with no significant disturbance from the major fluorescent reagent degradation by-products, such as 2(9-carbazole)-ethanol and bis-(2-(9-carbazole)-ethyl) carbonate. In addition, the detection responses for CEOC derivatives are compared to those obtained with FMOC. The ratios AC(CEOC)/AC(FMOC) = 1.00-1.82 for fluorescence (FL) response and AC'(CEOC)/AC'(FMOC) = 1.00-1.21 for ultraviolet (UV) response are observed (here, AC and AC' are, respectively, FL and UV F response). Separation of the derivatized peptides and amino acids has been optimized on a Hypersil BDS C18 column. Excellent linear responses are observed. This method was used successfully to analyze protein hydrolysates from wool and from direct-derivatized beer. (C) 2003 Elsevier Science (USA). All rights reserved.

Determination of 1-phenyl-3-methyl-5-pyrazolone-labeled carbohydrates by liquid chromatography and micellar electrokinetic chromatography

In this paper, the method for the derivatization of carbohydrates with 1-phenyl-3-methyl-5-pyrazolone (PMP) was simplified. One-third of the derivatization time was saved. Five monosaccharide derivatives have been well separated by MEKC and HPLC under optimized conditions. Good reproducibility could be obtained with relative standard deviation (RSD) values of the migration times within 5.0 and 2.3%, respectively. Furthermore, the developed methods have been successfully applied to the analysis of carbohydrates in Aloe powder and food. These methods are quite useful for routine analysis of monosaccharides and oligosaccharides in real samples. (C) 2003 Elsevier B.V. All rights reserved.

Determination of arsenic species by capillary zone electrophoresis with large-volume field-amplified stacking injection

Determination of arsenic species by large-volume field amplified stacking injection-capillary zone electrophoresis (LV-FASI-CZE) is reported in this paper. Whole column injection was employed. The optimum buffer pH for the separation of weak acids was discussed. It was found that the optimum buffer to analyze the stacked arsenate (As(V)), monomethylarsonate (MMA), and dimethylarsinate (DMA) was 25 mm phosphate at pH 6.5. However, the optimum buffer to analyze the concentrated arsenite (As(III)) was 20 mm phosphate - 10 mm borate at pH 9.28. The limits of detection of the method developed were 0.026 mg/L for As(III), 0.023 mg/L for As(V), 0.043 mg/L for MMA, and 0.018 mg/L for DMA. An enrichment factor of 34-100 for several arsenic species was obtained. In the end, this method was applied to determine the arsenic concentration in the environmental reference materials to show the usefulness of the method developed.

Direct determination of sialic acids in serum by capillary electrophoresis with UV detection

A novel method for the determination of N-acetylneuraminic acid (NANA) and N-glycolylneuraminic acid (NGNA) has been developed using high-performance capillary electrophoresis with UV detection at 195 nm, without pre or post-column derivatisation. The acids were separated in a 50-cm, fused-silica capillary (50 mu m i.d, 45.5-cm effective length) with Na2B4O7-Na2HPO4 buffer. The detection limit for NANA is a concentration of 9.6 x 10(-6) M or, in terms of mass: 3.879 x 10(-14) mol (39 fmol). This method is applicable to determination of NANA in normal human serum. The results were also compared with those of the colorimetrie method.

Automated voltammetric system for shipboard determination of metal speciation in sea water

An automated and semi-intelligent voltammetric system is described for trace metal analysis. The system consists of a voltammeter interfaced with a personal computer, a sample changer, 2 peristaltic pumps, a motor burette and a hanging mercury drop electrode. The system carries out fully automatically approximately 5 metal determinations per hour (including at least 3 repetitive scans and calibration by standard addition) at trace levels encountered in clean sea water. The computer program decides what level of standard addition to use and evaluates the data prior to switching to the next sample. Alternatively, the system can be used to carry out complexing ligand titration with copper whilst recording the labile copper concentration; in this mode up to 8 full titrations are carried out per day. Depth profiles for chromium speciation in the Mediterranean Sea and a profile for copper complexing ligand concentrations in the North Atlantic Ocean measured on board-ship with the system are presented. The chromium speciation was determined using a new method to differentiate between Cr(III) and Cr(VI) utilizing adsorption of Cr(III) on silica particles.

Determination of photochemically produced hydroxyl radicals in seawater and freshwater

A variety of short-lived, reactive chemical species (i.e. free radicals and excited state species) are known to be photochemically produced in natural waters. Some of these transients may strongly affect chemical and biological processes, and they have been implicated in the degradation of organic pollutants and natural organic compounds in aqueous environments. Previous studies demonstrated that the highly reactive hydroxyl radical (OH) is photochemically formed in seawater. However, the quantitative importance of this key species in the sea has not been previously studied because of past analytical limitations. By using a highly sensitive probe based on α-H atom abstraction from methanol, we were able to measure production rates and steady-state concentrations of photochemically produced OH radicals in coastal and open ocean seawater and freshwaters. The validity of the method was tested by intercalibrating with an independent, OH-specific reaction, hydroxylation of benzoic acid, and also by competition kinetics experiments. Our OH production rates and steady-state concentrations for freshwaters are in excellent agreement with those measured by previous investigators for similar waters. In contrast, for seawater, the values we measured are 1–3 orders of magnitude higher than previously predicted by models, indicating that there is a major unknown photochemical OH source (s) in seawater.