Small Internal Diameter Research Articles

A simplified and efficient method for the analysis of fatty acid methyl esters suitable for large clinical studies

Conventional sample preparation for fatty acid analysis is a complicated, multiple-step process, and gas chromatography (GC) analysis alone can require >1 h per sample to resolve fatty acid methyl esters (FAMEs). Fast GC analysis was adapted to human plasma FAME analysis using a modified polyethylene glycol column with smaller internal diameters, thinner stationary phase films, increased carrier gas linear velocity, and faster temperature ramping. Our results indicated that fast GC analyses were comparable to conventional GC in peak resolution. A conventional transesterification method based on Lepage and Roy was simplified to a one-step method with the elimination of the neutralization and centrifugation steps. A robotics-amenable method was also developed, with lower methylation temperatures and in an open-tube format using multiple reagent additions. The simplified methods produced results that were quantitatively similar and with similar coefficients of variation as compared with the original Lepage and Roy method. The present streamlined methodology is suitable for the direct fatty acid analysis of human plasma, is appropriate for research studies, and will facilitate large clinical trials and make possible population studies.

SU‐FF‐T‐153: Influence of Ionization Chamber Size for Intensity Modulation Treatment Planning Modeling

Purpose: Intensity modulation treatment planning systems (TPS) modeling requiere beam data collection of depth dose curves and dose profiles for open fields. The internal ionization chamber diameter is related with the width of the penumbra. The purpose of this work is to model a photon beam for Intensity Modulation Radiotherapy (IMRT) using two chambers with different sizes and compare the modeling results with film measurements using standard dynamic IMRT patterns. Method and Materials: The TPS used was CadPlan/Helios. The treatment energy used was 6 MeV generated by a linear accelerator Clinac 21EX equipped with a 120‐leaf multileaf (MLC). The ionization chambers used were Wellhofer IC‐10 (0.14cc) with internal diameter of 6 mm and a PTW Pint Point 31014 (0.015cc) with an internal diameter of 2 mm. Five standards IMRT patterns were used for comparisson. Grid calculation size was 2.5×2.5 mm2 and 1.25×1.25 mm2. To match calculated to film‐measured isodoses, external MLC generated registration points were used. Measured isodoses were done using Kodak EDR2 film. Comparisson between calculated and measured isodoses were done by gamma evaluation (3mm/3% and 2mm/2%) using RIT113 software. Results: Measurements of dose profiles with Pint Point detector showed narrower penumbra (20%–80% penumbra width at 5 cm depth in water were 4.0 mm for the Pint Point chamber and 6.0 mm with the IC‐10). Detector noise and measuring time increased with Pint Point chamber. Single pencil beam kernels generated from profiles measurements at 5 depths were sharper with the Pint Point detector. Agreement between calculated and measured isodoses was better with the smaller detector in all the standard IMRT patterns, especially at the high dose gradient regions. Conclusions: For CadPlan/Helios TPS, beam modeling for IMRT improves using an ionization chamber with smaller internal diameter.

Capillary columns in liquid chromatography: between conventional columns and microchips

Liquid chromatography on columns with small internal diameters has been reviewed as the intermediate technique between conventional liquid chromatography and microchip separations. The development of micro column separations in the early years has been described, starting with the papers of Horváth and co-workers and Ishii and co-workers, continuing into the first part of the eighties, then making a leap in time to recent innovations with small-bore columns. Based on internal diameters a classification of the different analytical HPLC columns has been suggested. The advantages of small-bore columns have been discussed, with particular emphasis on the advantage of coupling to concentration sensitive detectors when the sample amount is limited. Open tubular columns are treated as a part of the historic background. The recent developments include a brief look into the current status of monolithic columns, the use of packed nano columns and micro columns with electrospray mass spectrometry, and the potential of two-dimensional comprehensive liquid chromatography. Finally, the coupling of sample preparation to analytical columns and the future applications of the novel technological improvements to the microchip separation methods have been discussed.

Anterior adhesive areas and adjacent secretions in the parasitic flatworms Decacotyle lymmae and D. tetrakordyle (Monogenea: Monocotylidae) from the gills of stingrays

Abstract. The monogeneans Decacotyle lymmae and D. tetrakordyle (Monocotylidae: Decacotylinae), from gills of the dasyatid stingrays Taeniura lymma and Pastinachus sephen, respectively, have a single aperture for adhesive secretion on each side of the anterior ventrolateral region. Rod‐shaped bodies (S1) and electron‐dense spherical secretion (S2) exit through specialised ducts opening adjacent to one another within these apertures. The S1 bodies are 230 ± 11 nm wide and ≥4 μm long in D. lymmae and 240 ± 9 nm wide and ≥3.3 μm long in D. tetrakordyle. The S2 bodies have a diameter of 88 ± 7 nm in D. lymmae and 65 ± 6 nm in D. tetrakordyle. The apertures are unusual in being extremely small (internal diameter, 3–5 μm). Each aperture has a slit‐like surface opening as small as 160 nm wide, surrounded by muscle fibres indicating that they may be opened and closed. The aperture is also surrounded and underlain by muscle fibres that may aid in secretion from, or even eversion of, the tissue within the aperture. Sensilla/cilia are also found within the apertures. Additional secretions from anteromedian and anterolateral glands (body glands), each containing granular secretions, occur in profusion and exit anteriorly and posteriorly to the position of the apertures, through duct openings in the general body tegument. These granular secretions do not appear to be associated with anterior adhesion. Both species show similarities in aperture, underlying tissue, sense organ, and secretion detail, in accordance with findings from other monogenean genera, and which supports the importance of such data for phylogenetic studies.

Rotational in vitro compliance measurement of diverse anastomotic configurations: a tool for anastomotic engineering

Anastomotic configurations with a small internal diameter are prone to intimal hyperplasia which can cause occlusion within weeks or months. A link between intimal hyperplasia and inhomogenities of the elastic profile of the anastomosis has been established, making anastomotic engineering directed towards smoothing the compliance profile at the anastomotic site essential. Methods to date restrict the anastomotic compliance measurement to one plane. We present a method by which the anastomotic configurations are rotated, thereby allowing an anastomotic elastic profile assessment in multiple planes. Eight end-to-end anastomoses (ovine common carotid artery) and three end-to-side anastomoses (e-PTFE graft to ovine common carotid artery) were prepared and mounted in an artificial circulation system. Anastomotic circumferential compliance (maximal–minimal diameter/(maximal–minimal pressure·minimal diameter)) was measured by means of a laser-scan-micrometer and a Statham pressure transducer. By rotating end-to-end anastomoses, the compliance was measured in three, and in end-to-side anastomoses in four different planes. Multiplanar compliance variability in areas remote to both end-to-end and end-to-side anastomoses was approximately 9%. At the suture line the variability was approximately 22% in end-to-end anastomoses and 78% in end-to-side anastomoses. These results show that local factors result in different compliance profiles when utilizing a multiplanar technique, particularly in end-to-side anastomoses. The rotational apparatus is a tool which can be used to more accurately engineer a homogeneously compliant anastomosis, with the ultimate goal of prolonging anastomotic patency.

Multi-reflection photometric flow cell for use in flow injection analysis of estuarine waters

A multi-reflection flow cell suitable for flow analysis is described. Light from an LED is directed through an optical fibre into a silver coated capillary through a sidewall aperture, and emerges through a similar aperture 10 mm along the capillary after undergoing an estimated 19 reflections. This process provides a sensitivity enhancement of approximately 2.5 compared with a conventional z-cell of the same nominal path length. This enhancement is due to both the increased optical path length achieved by multiple reflection of the light beam through the sample, and minimization of physical dispersion by the use of a short, small internal diameter capillary as the flow cell. The optical design of this flow cell also minimizes the Schlieren effect. Optical and hydrodynamic characteristics of this multi-reflection cell have been evaluated using a series of bromothymol blue dye studies. Application of the flow cell to the determination of reactive phosphorus in estuarine waters with wide variation in salinity and refractive index is also described.

Infrared Multiphoton Dissociation with a Hollow Fiber Waveguide

A novel scheme for performing infrared multiphoton dissociation (IRMPD) is presented in which a hollow fiber waveguide (HFWG) is used to transmit IR radiation into the ion storage region of a mass spectrometer. Efficient dissociation of oligonucleotide and protein ions is demonstrated on an ESI-FTICR instrument in which IRMPD is performed in the external ion reservoir and on a quadrupole ion trap. Using a simple optical scheme consisting of a single focusing lens and an x, y translator, the 10.6-microm IR laser beam, initially 3.5 mm in diameter, is focused into the vacuum-sealed HFWG. The small internal diameter and the high transfer efficiency of the waveguide allow IR radiation of high power density to be employed for IRMPD. In studies performed on a quadrupole ion trap, a 500-microm-i.d. waveguide was used as a medium to transmit IR radiation directly through a 700-microm orifice in the ring electrode. Efficient IRMPD of both a 12-mer oligonucleotide and the protein melittin were performed at laser powers of 0.5 and 3.2 W, respectively.

Variety of the molecular conformation in Peptide nanorings and nanotubes.

Possible molecular conformations in peptide nanorings and nanotubes were theoretically investigated by a mathematical conformation analysis as well as ab initio Hartree-Fock calculations. The mathematical analysis predicts not only the conventional nanorings having an extended-type (E-type) backbone (trans zigzag) but also the novel ones having bound-type (B-type) backbones with a smaller internal diameter. Ab initio calculations for the amino acid substitution reveal that all 20 encoded residues can form both types of the above nanorings as a local minimum. However, the energetically stable type is determined in accordance with the kind of the replaced side chains. Moreover, the present work theoretically reveals that both types of nanorings stack to form nanotubes through inter-ring hydrogen bonds, i.e., larger E-type nanotubes and smaller B-type nanotubes. Electronically, the HOMO and LUMO states of the nanoring and nanotube backbones are formed by the in-plane pi state. The replacement by the appropriate residues is furthermore predicted to intrude additional levels in the energy gap and to form the frontier states localized at the side chains.

Relationship Between Internal Phase Volume and Emulsion Stability: The Cetyl Alcohol/Stearyl Alcohol System

The main objective of this study was to optimize the stability of cetyl alcohol/stearyl alcohol emulsions in terms of percentage of internal phase volume, emulsifier type and concentration, and amount of external phase (water). Creams (o/w emulsions) were prepared by phase inversion and physical properties as particle size of the internal phase, apparent viscosity, and sedimentation volume evaluated. Stability was performed at room temperature, 40°C, 50°C, and under stress conditions. High hydrophilic lipophilic balance (HLB) nonionic surfactants as tween 80, tween 20, Myrj 52, Brij 35, and low HLB span 60 were used as emulsifying agents. The percentage of internal phase components (cetyl alcohol and stearyl alcohol), percentage of emulsifying agents, and percentage of aqueous external phase were varied, and stability was investigated. As the level of emulsifier agent (tween 80 and span 60) increased from 3% to 15%, and the percent of the internal phase remained constant at 30%, the particle size of the internal phase decreased and the cream became more stable. Formulations of the same composition, but prepared using Myrj 53 and tween 20 as emulsifiers, showed a larger particle size than formulations prepared using tween 80 and Brij 35. As the level of the internal phase volume increased and consequently the amount of water decreased, emulsion viscosity increased. The best formulation containing 30% internal phase (50% cetyl alcohol, 35% stearyl alcohol), 15% emulsifying agents (tween 80/span 60 ratio of 3:1), and 70% water was selected, and effects of process temperature and cooling rate on emulsion stability investigated. This formulation was further investigated in terms of stability of a 1% hydrocortisone addition by varying the percentage (30%, 35%, 40%, and 45%) of internal phase and percentage of water (70%, 65%, 60%, and 55%). The best formulation contained 45% internal phase (22.5 g cetyl alcohol, 15.75 g stearyl alcohol, 15% emulsifying agent, which is equivalent to 5 g tween 80 and 1.7 g span 60), and 55% w/w water, was manufactured under different manufacturing processes. Emulsions prepared by homogenization at the beginning of the process of emulsification were stable with small internal phase particle diameter. This study demonstrates that at every cetyl alcohol/stearyl alcohol ratio there is a phase volume/emulsifier HLB ratio, which results in optimum stability.

Low-frequency Raman studies of multiwalled carbon nanotubes: Experiments and theory

In this paper, we investigate the low frequency Raman spectra of multiwalled carbon nanotubes (MWNT's) prepared by the electric arc method. Low frequency Raman modes are unambiguously identified on purified samples thanks to the small internal diameter of the MWNT's. We propose a model to describe these modes. They originate from the radial breathing vibrations of the individual walls coupled through the van der Waals interaction between adjacent concentric walls. The intensity of the modes is described in the framework of bond polarization theory. Using this model and the structural characteristics of the nanotubes obtained from transmission electron microscopy, we simulated the experimental low frequency Raman spectra with excellent agreement. Therefore Raman spectroscopy can be as useful in the characterization of MWNT's as it is for single-wall nanotubes.

Modification of a commercial electrospray nebulizer for operation in a liquid chromatography/mass spectrometry system at flow rates in the low microL/min range.

A simple and inexpensive approach to convert the electrospray nebulizer of a commercial liquid chromatography/mass spectrometry (LC/MS) system (HP 1100) to accommodate lower flow rates has been proposed and evaluated. This modification consists of simply replacing the nebulizer needle by a commercially available stainless steel needle with a smaller internal diameter. Experiments were conducted in order to optimize operational parameters. Using two different internal diameter needle sizes, flow rates ranging from 1 to 250 microL/min could be accommodated. The modification presented allows an extension of the range of compatible flow rates without major modification of the standard design of the interface.

Recent progress in enantiomer separation by capillary electrochromatography

Enantiomer separation by electrochromatography (CEC) can be performed in three modes: (i) open-tubular capillary electrochromatography (o-CEC), in which the chiral selector is physically adsorbed coated, and thermally immobilized or covalently attached to the internal capillary wall; (ii) packed capillary electrochromatography (p-CEC), in which the capillary is either filled with chiral modified silica particles or with an achiral packing material, and a chiral selector is added to the mobile phase; and (iii) monolithic (rod)-capillary electrochromatography (rod-CEC) in which the chiral stationary phase (CSP) consists of a single piece of porous solid. We present an overview on methods and new trends in the field of electrochromatographic enantiomer separation such as CEC with either nonaqueous mobile phases or stationary phases with incorporated permanent charges, or with packing beds consisting of nonporous silica particles or particles with very small internal diameters.

Comparison of first- and second-generation prostheses for endoluminal repair of abdominal aortic aneurysms: A 6-year study with life table analysis

Purpose: The outcome of endoluminal repair of abdominal aortic aneurysms with two generations of prostheses was analyzed and compared. Methods: Between May 1992 and December 1998, 266 patients underwent elective endoluminal repair of an AAA. First-generation prostheses were used in 118 patients (group I), and second-generation prostheses were used in 148 patients (group II). The two groups were similar in age, sex, and size of AAA. The proportion of patients with comorbidities was higher in group I than in group II, but not significantly. First-generation devices were characterized by large (24F internal diameter) delivery systems, one-piece construction, and a lack of metallic support throughout their length. Second-generation devices had smaller (21F or smaller internal diameter) delivery systems, modular construction, and a metallic frame throughout the length of the prostheses. The major end-point criteria were survival and successful endoluminal repair. Success was defined as the exclusion of the aneurysm sac from the circulation, with stability or the reduction in AAA maximum transverse diameter. Persistent endoleaks were classified as failures, irrespective of whether they were subsequently corrected by means of secondary endovascular intervention. The minimum follow-up period was 5 months for each of the 266 patients. Analysis was performed by means of the life-table method. Results: Perioperative mortality was not significantly different between group I (4.2%) and group II (2.7%). There was a statistically significant difference between the survival curves of the two generations, which favored group II (P =.012). There was a significant (P <.001) difference between the two generations of patients in their conditional probability of graft failure when the competing risk of all-cause mortality was considered. Second-generation patients were at a lower risk of graft failure than first-generation patients. The probability of failure, expressed as a proportion of grafts failing at 2 years, was 0.15 for patients with second-generation prostheses and 0.33 for patients with first-generation prostheses. Conclusion: Endoluminal AAA repair is a safe procedure, whether first- or second-generation prostheses are used. Survival and probability of graft success were significantly higher with second-generation prostheses than with first-generation prostheses. This improvement in outcome resulted from a combination of increasing clinical experience and advances in technology. A more accurate evaluation of the role of the endoluminal method in AAA repair would be achieved by studying patients in whom second-generation devices were used, rather than longer term studies in which first- and second-generation devices were used. (J Vasc Surg 2000;32:124-9.)

Split-flow injector for capillary zone electrophoresis

A simple construction of a split-flow injector eliminating some common problems connected with the use of such devices is described. It consists of a low-pressure pump, an injection valve and a delivery tube in which the separating capillary inlet is fixed. The sample is injected without moving the separating capillary inlet and without interrupting the applied voltage. The grounded electrophoretic electrode is close to the injection valve so that all metal parts of the injector are kept at a sufficiently low potential. Minimum length and small internal diameter of delivery tube minimizes additional sample zone broadening. The effects of some experimental parameters, such as the position of the separation capillary inlet with respect to the background solution flow direction and background solution flow-rate are experimentally studied. The injector was tested primarily for the electrokinetic injection.

Duplex scanning to assess radial artery suitability for coronary artery bypass grafting.

Radial artery suitability in coronary artery bypass grafting was assessed using duplex ultrasonography. The vascular condition along the entire radial artery was scanned in 55 patients, measuring the internal diameter and mean flow velocity at the wrist (distally), after ulnar artery branching (proximally), and midway between these 2 points (medially). Distally along the radial and ulnar arteries, the mean flow velocity was determined before and after radial artery occlusion. Atherosclerotic changes were detected in 4 patients. The internal diameter was 3.1 +/- 0.4 mm proximally, 2.7 +/- 0.3 mm medially, 2.4 +/- 0.4 mm distally. The distal flow velocity was 0, and a reverse flow (peak velocity: 11.3 +/- 6.0 cm/s) was observed after the occlusion test in patients with an intact palmar arch, their mean flow velocity, 21.1 +/- 8.9 cm/s, and flow distally along the ulnar artery 58.0 +/- 23.4 ml/min, were higher after the occlusion test than before it 14.7 +/- 6.7 cm/s mean flow and 38.1 +/- 15.9 ml/min distally. This was not observed in patients with an interrupted palmar arch. In 15 patients, radial arteries could not be used because of their small internal diameter, lack of a radial artery, poor vascular condition, or an interrupted palmar arch evaluated using duplex scanning. Reliable noninvasive assessment of radial artery anatomy and palmar arch continuity is thus possible using duplex ultrasonography.

Quasi-linear gradients for capillary liquid chromatography with mass and tandem mass spectrometry.

Gradient elution, capillary liquid chromatography mass spectrometry was performed with linear, static gradients constructed by laminar flowing ten, 1.5 microL volume steps of decreasing organic concentration into tubing of small internal diameter. Sample loading, gradient formation, and sample elution were accomplished entirely by means of a commercially available micro-autosampler and single-syringe drive pump. The procedure was simple, fast, stable, and reproducible. Essentially linear gradients were produced without the use of additional valves, mixers, pumps or software. It took less than 10 minutes to form a gradient and less than 30 minutes to construct the set of individual buffer vials. The gradients were shown to be stable to storage. One hour after forming, peak retention times were reproduced to +/-0.5%. Long-term retention time reproducibility was found to vary by +/-2%. Chromatographic resolution was comparable or superior to that obtained by gradient elution with conventional dynamic mixing and split flow. The procedure was adapted with a 'peak parking' method which extended the time for generating peptide fragmentation data up to 10 minutes per peptide with the triple quadruple mass spectrometer. Using this technique, collision data were collected at the 25 femtomole level on nine of ten tryptic peptides in a single run.

The visceral perfusion system and distal bypass during thoracoabdominal aneurysm surgery: an alternative for physiological blood flow?

There are potential benefits to addition of visceral organ perfusion, by means of a 9-Fr. catheter system (octopus), to distal aortic perfusion during thoracoabdominal aneurysm surgery. However, in the literature there are reports of adverse effects. The authors therefore compared two groups of patients who underwent thoracoabdominal aneurysm surgery with and without visceral organ perfusion. In the group in which the visceral perfusion was applied, the use of platelets (26 versus 11 units; P<0.05), fresh frozen plasma (3.4 versus 1.5 units; P<0.05) and packed cells (20 versus 8 units, P<0.05) was significantly increased. An equal number of patients in both groups developed renal failure postoperatively. An explanation for this adverse effect can be found in the high shear rates in the catheters used, mainly as a result of the small diameter. High shear rates cause haemolysis. Also, the flow through the catheters is insufficient to maintain adequate perfusion of the visceral organs. A higher flow in these catheters would result in an even higher shear rate. It is therefore concluded that coagulopathy and insufficient bloodflow is caused by the small internal diameter of the catheters, which renders the device insufficient.

The Visceral Perfusion System and Distal Bypass during Thoracoabdominal Aneurysm Surgery: An Alternative for Physiological Blood Flow?

There are potential benefits to addition of visceral organ perfusion, by means of a 9-Fr. catheter system (octopus), to distal aortic perfusion during thoracoabdominal aneurysm surgery. However, in the literature there are reports of adverse effects. The authors therefore compared two groups of patients who underwent thoracoabdominal aneurysm surgery with and without visceral organ perfusion. In the group in which the visceral perfusion was applied, the use of platelets (26 versus 11 units; P &lt; 0.05), fresh frozen plasma (3.4 versus 1.5 units: P &lt; 0.05) and packed cells (20 versus 8 units, P &lt; 0.05) was significantly increased. An equal number of patients in both groups developed renal failure postoperatively. An explanation for this adverse effect can be found in the high shear rates in the catheters used, mainly as a result of the small diameter. High shear rates cause haemolysis. Also, the flow through the catheters is insufficient to maintain adequate perfusion of the visceral organs. A higher flow in these catheters would result in an even higher shear rate. It is therefore concluded that coagulopathy and insufficient bloodflow is caused by the small internal diameter of the catheters, which renders the device insufficient.

Hollow cathode sputtering cluster source for low energy deposition: Deposition of Fe small clusters

We have developed a new cluster deposition source, which can be applied to the formation of nanostructured thin films. By our method, clusters are created by a hollow cathode sputtering at high pressure in the range of hundreds of Pa, which are directly deposited onto substrates. A pipe target with small internal diameter of 6 mm is used, and He is injected as a carrier gas while using Ar as a sputtering gas. The cluster size can be controlled between 2 and 6 nm in diameter, and high deposition rates up to 25 nm/min for 6 nm Fe clusters are obtained on a considerably wide substrate. It is also demonstrated that the deposition of 6 nm Fe clusters produces continuous films consisting of very small grains of nearly the same size with depositing clusters.

An ion funnel interface for improved ion focusing and sensitivity using electrospray ionization mass spectrometry.

To improve upon the already impressive sensitivity achievable with electrospray ionization sources, a novel electrohydrodynamic ion funnel interface has been developed and implemented with a triple-quadrupole mass spectrometer. The ion funnel interface effectively consists of a series of ring electrodes of increasingly small internal diameters to which rf and dc electric potentials are coapplied. In the 1-10-Torr pressure range, the electric fields cause the collisionally damped ions to be more effectively focused and transmitted as a collimated ion beam. This paper describes the ion funnel design and presents an evaluation of its performance using a triple-quadrupole mass spectrometer. Ion transmission and m/z discriminating parameters (resulting in both effective low- and high-m/z cutoffs) are presented based upon both ion current measurements and mass spectra. Electrospray ionization mass spectra of selected protein solutions demonstrated well over 1 order of magnitude increase in signal relative to that of the instrument operated in its standard (inlet capillary-skimmer) configuration under similar conditions. The present results suggest that it will be feasible to realize close to 100% ion transmission efficiency for analytically relevant ions through the electrospray ionization interface and into the mass analyzer.