High efficient extraction of M@C-2n (M = La, Ce) by a high pressure and high temperature method

A high pressure and high temperature method was used to efficiently extract on a large scale metallofullerenes M@C-2n (M=La,Ce) in a closed vessel under argon gas protection. With pyridine as the HPHT solvent, about 60-80% M@C-2n and 30-55% M@C-82 can be enriched, M@C-82 is dissolved selectively; With toluene as the HPHT solvent, M@C-2n can also be efficiently extracted, especially M@C-74, which is a new member of M@C-2n soluble species. (C) 1998 Elsevier Science Ltd. All rights reserved.

A new and improved strategy combining a dispersive-solid phase extraction-based multiclass method with ultra high pressure liquid chromatography for analysis of low molecular weight polyphenols in vegetables

This paper reports on the development and optimization of a modified Quick, Easy, Cheap Effective, Rugged and Safe (QuEChERS) based extraction technique coupled with a clean-up dispersive-solid phase extraction (dSPE) as a new, reliable and powerful strategy to enhance the extraction efficiency of free low molecular-weight polyphenols in selected species of dietary vegetables. The process involves two simple steps. First, the homogenized samples are extracted and partitioned using an organic solvent and salt solution. Then, the supernatant is further extracted and cleaned using a dSPE technique. Final clear extracts of vegetables were concentrated under vacuum to near dryness and taken up into initial mobile phase (0.1% formic acid and 20% methanol). The separation and quantification of free low molecular weight polyphenols from the vegetable extracts was achieved by ultrahigh pressure liquid chromatography (UHPLC) equipped with a phodiode array (PDA) detection system and a Trifunctional High Strength Silica capillary analytical column (HSS T3), specially designed for polar compounds. The performance of the method was assessed by studying the selectivity, linear dynamic range, the limit of detection (LOD) and limit of quantification (LOQ), precision, trueness, and matrix effects. The validation parameters of the method showed satisfactory figures of merit. Good linearity (View the MathML sourceRvalues2>0.954; (+)-catechin in carrot samples) was achieved at the studied concentration range. Reproducibility was better than 3%. Consistent recoveries of polyphenols ranging from 78.4 to 99.9% were observed when all target vegetable samples were spiked at two concentration levels, with relative standard deviations (RSDs, n = 5) lower than 2.9%. The LODs and the LOQs ranged from 0.005 μg mL−1 (trans-resveratrol, carrot) to 0.62 μg mL−1 (syringic acid, garlic) and from 0.016 μg mL−1 (trans-resveratrol, carrot) to 0.87 μg mL−1 ((+)-catechin, carrot) depending on the compound. The method was applied for studying the occurrence of free low molecular weight polyphenols in eight selected dietary vegetables (broccoli, tomato, carrot, garlic, onion, red pepper, green pepper and beetroot), providing a valuable and promising tool for food quality evaluation.

Rapid and sensitive ultra-high-pressure liquid chromatography method for quantification of antichagasic benznidazole in plasma: application in a preclinical pharmacokinetic study

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

The relationship between measurement method and corneal structure on apparent intraocular pressure in glaucoma and ocular hypertension

Purpose: To analyse the relationship between measured intraocular pressure (IOP) and central corneal thickness (CCT), corneal hysteresis (CH) and corneal resistance factor (CRF) in ocular hypertension (OHT), primary open-angle (POAG) and normal tension glaucoma (NTG) eyes using multiple tonometry devices. Methods: Right eyes of patients diagnosed with OHT (n=47), normal tension glaucoma (n=17) and POAG (n=50) were assessed, IOP was measured in random order with four devices: Goldmann applanation tonometry (GAT); Pascal(R) dynamic contour tonometer (DCT); Reichert(R) ocular response analyser (ORA); and Tono-Pen(R) XL. CCT was then measured using a hand-held ultrasonic pachymeter. CH and CRF were derived from the air pressure to corneal reflectance relationship of the ORA data. Results: Compared to the GAT, the Tonopen and ORA Goldmann equivalent (IOPg) and corneal compensated (IOPcc) measured higher IOP readings (F=19.351, p<0.001), particularly in NTG (F=12.604, p<0.001). DCT was closest to Goldmann IOP and had the lowest variance. CCT was significantly different (F=8.305, p<0.001) between the 3 conditions as was CH (F=6.854, p=0.002) and CRF (F=19.653, p<0.001). IOPcc measures were not affected by CCT. The DCT was generally not affected by corneal biomechanical factors. Conclusion: This study suggests that as the true pressure of the eye cannot be determined non-invasively, measurements from any tonometer should be interpreted with care, particularly when alterations in the corneal tissue are suspected.

A novel method for rapid and selective extraction of male DNA from rape kits using alkaline lysis and pressure cycling technology (PCT)

There is an increasing demand for DNA analysis because of the sensitivity of the method and the ability to uniquely identify and distinguish individuals with a high degree of certainty. But this demand has led to huge backlogs in evidence lockers since the current DNA extraction protocols require long processing time. The DNA analysis procedure becomes more complicated when analyzing sexual assault casework samples where the evidence contains more than one contributor. Additional processing to separate different cell types in order to simplify the final data interpretation further contributes to the existing cumbersome protocols. The goal of the present project is to develop a rapid and efficient extraction method that permits selective digestion of mixtures. ^ Selective recovery of male DNA was achieved with as little as 15 minutes lysis time upon exposure to high pressure under alkaline conditions. Pressure cycling technology (PCT) is carried out in a barocycler that has a small footprint and is semi-automated. Typically less than 10% male DNA is recovered using the standard extraction protocol for rape kits, almost seven times more male DNA was recovered from swabs using this novel method. Various parameters including instrument setting and buffer composition were optimized to achieve selective recovery of sperm DNA. Some developmental validation studies were also done to determine the efficiency of this method in processing samples exposed to various conditions that can affect the quality of the extraction and the final DNA profile. ^ Easy to use interface, minimal manual interference and the ability to achieve high yields with simple reagents in a relatively short time make this an ideal method for potential application in analyzing sexual assault samples.^

Study of the calibration method of pressure-velocity probes and its application in a field of progressive plane waves

This dissertation presents a calibration procedure for a pressure velocity probe. The dissertation is divided into four main chapters. The first chapter is divided into six main sections. In the firsts two, the wave equation in fluids and the velocity of sound in gases are calculated, the third section contains a general solution of the wave equation in the case of plane acoustic waves. Section four and five report the definition of the acoustic impedance and admittance, and the practical units the sound level is measured with, i.e. the decibel scale. Finally, the last section of the chapter is about the theory linked to the frequency analysis of a sound wave and includes the analysis of sound in bands and the discrete Fourier analysis, with the definition of some important functions. The second chapter describes different reference field calibration procedures that are used to calibrate the P-V probes, between them the progressive plane wave method, which is that has been used in this work. Finally, the last section of the chapter contains a description of the working principles of the two transducers that have been used, with a focus on the velocity one. The third chapter of the dissertation is devoted to the explanation of the calibration set up and the instruments used for the data acquisition and analysis. Since software routines were extremely important, this chapter includes a dedicated section on them and the proprietary routines most used are thoroughly explained. Finally, there is the description of the work that has been done, which is identified with three different phases, where the data acquired and the results obtained are presented. All the graphs and data reported were obtained through the Matlab® routine. As for the last chapter, it briefly presents all the work that has been done as well as an excursus on a new probe and on the way the procedure implemented in this dissertation could be applied in the case of a general field.

A Novel Method for Rapid and Selective Extraction of Male DNA from Rape Kits using Alkaline Lysis and Pressure Cycling Technology (PCT)

There is an increasing demand for DNA analysis because of the sensitivity of the method and the ability to uniquely identify and distinguish individuals with a high degree of certainty. But this demand has led to huge backlogs in evidence lockers since the current DNA extraction protocols require long processing time. The DNA analysis procedure becomes more complicated when analyzing sexual assault casework samples where the evidence contains more than one contributor. Additional processing to separate different cell types in order to simplify the final data interpretation further contributes to the existing cumbersome protocols. The goal of the present project is to develop a rapid and efficient extraction method that permits selective digestion of mixtures. Selective recovery of male DNA was achieved with as little as 15 minutes lysis time upon exposure to high pressure under alkaline conditions. Pressure cycling technology (PCT) is carried out in a barocycler that has a small footprint and is semi-automated. Typically less than 10% male DNA is recovered using the standard extraction protocol for rape kits, almost seven times more male DNA was recovered from swabs using this novel method. Various parameters including instrument setting and buffer composition were optimized to achieve selective recovery of sperm DNA. Some developmental validation studies were also done to determine the efficiency of this method in processing samples exposed to various conditions that can affect the quality of the extraction and the final DNA profile. Easy to use interface, minimal manual interference and the ability to achieve high yields with simple reagents in a relatively short time make this an ideal method for potential application in analyzing sexual assault samples.

The development of an algorithm to track blood pressure accurately based on the pulse transit time method

Oscillometric blood pressure (BP) monitors are currently used to diagnose hypertension both in home and clinical settings. These monitors take BP measurements once every 15 minutes over a 24 hour period and provide a reliable and accurate system that is minimally invasive. Although intermittent cuff measurements have proven to be a good indicator of BP, a continuous BP monitor is highly desirable for the diagnosis of hypertension and other cardiac diseases. However, no such devices currently exist. A novel algorithm has been developed based on the Pulse Transit Time (PTT) method, which would allow non-invasive and continuous BP measurement. PTT is defined as the time it takes the BP wave to propagate from the heart to a specified point on the body. After an initial BP measurement, PTT algorithms can track BP over short periods of time, known as calibration intervals. After this time has elapsed, a new BP measurement is required to recalibrate the algorithm. Using the PhysioNet database as a basis, the new algorithm was developed and tested using 15 patients, each tested 3 times over a period of 30 minutes. The predicted BP of the algorithm was compared to the arterial BP of each patient. It has been established that this new algorithm is capable of tracking BP over 12 minutes without the need for recalibration, using the BHS standard, a 100% improvement over what has been previously identified. The algorithm was incorporated into a new system based on its requirements and was tested using three volunteers. The results mirrored those previously observed, providing accurate BP measurements when a 12 minute calibration interval was used. This new system provides a significant improvement to the existing method allowing BP to be monitored continuously and non-invasively, on a beat-to-beat basis over 24 hours, adding major clinical and diagnostic value.

An approximate method for the solution of an influence function foil rolling model

Fleck and Johnson (Int. J. Mech. Sci. 29 (1987) 507) and Fleck et al. (Proc. Inst. Mech. Eng. 206 (1992) 119) have developed foil rolling models which allow for large deformations in the roll profile, including the possibility that the rolls flatten completely. However, these models require computationally expensive iterative solution techniques. A new approach to the approximate solution of the Fleck et al. (1992) Influence Function Model has been developed using both analytic and approximation techniques. The numerical difficulties arising from solving an integral equation in the flattened region have been reduced by applying an Inverse Hilbert Transform to get an analytic expression for the pressure. The method described in this paper is applicable to cases where there is or there is not a flat region.

The costs arising from pressure ulcers attributable to malnutrition

Aim To estimate the economic consequences of pressure ulcers attributable to malnutrition. Method Statistical models were developed to predict the number of cases of pressure ulcer, associated bed days lost and the dollar value of these losses in public hospitals in 2002/2003 in Queensland, Australia. The following input parameters were specified and appropriate probability distributions fitted • Number of at risk discharges per annum • Incidence rate for pressure ulcer • Attributable fraction of malnutrition in the development of pressure ulcer • Independent effect of pressure ulcer on length of hospital stay • Opportunity cost of hospital bed day One thousand random re-samples were made and the results expressed as (output) probabilistic distributions. Results The model predicts a mean 16060 (SD 5 671) bed days lost and corresponding mean economic cost of AU$12 968 668 (SD AU$4 924 148) (EUROS 6 925 268 SD 2 629 495; US$ 7 288 391 SD 2 767 371) of pressure ulcer attributable to malnutrition in 2002/2003 in public hospitals in Queensland, Australia. Conclusion The cost of pressure ulcer attributable to malnutrition in bed days and dollar terms are substantial. The model only considers costs of increased length of stay associated with pressure ulcer and not other factors associated with care.

Statistical modeling to determine resonant frequency information present in combustion chamber pressure signals

A statistical modeling method to accurately determine combustion chamber resonance is proposed and demonstrated. This method utilises Markov-chain Monte Carlo (MCMC) through the use of the Metropolis-Hastings (MH) algorithm to yield a probability density function for the combustion chamber frequency and find the best estimate of the resonant frequency, along with uncertainty. The accurate determination of combustion chamber resonance is then used to investigate various engine phenomena, with appropriate uncertainty, for a range of engine cycles. It is shown that, when operating on various ethanol/diesel fuel combinations, a 20% substitution yields the least amount of inter-cycle variability, in relation to combustion chamber resonance.