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PubMed2002

Evaluation of a high-resolution time-of-flight mass spectrometer for the gas chromatographic determination of selected environmental contaminants.

A benchtop high-resolution time-of-flight mass spectrometer (TOF MS) was evaluated for the determination of key organic microcontaminants. The major advantage of the TOF MS proved to be the high mass resolution of about 0.002 Da (10 ppm). Consequently, the detectability of polar pesticides, polynuclear aromatic hydrocarbons and polychlorinated biphenyls is excellent, and detection limits are in the order of 1-4 pg injected mass. Best mass spectral resolution was obtained for medium-scale peaks. It is a disadvantage that the calibration range is rather limited, viz. to about two orders of magnitude. The high mass spectral resolution was especially useful to improve the selectivity and sensitivity when analyzing target compounds in complex samples and to prevent false-positive identifications.

Calibration↗

PubMed2003

Effect of chromatographic conditions on resolution in high-performance ion-exchange chromatography of proteins on nonporous support.

We explored chromatographic conditions to obtain high resolution in protein separations by ion-exchange chromatography (IEC) on a nonporous anion-exchange resin of 2.5 microm in particle diameter. We studied the effects of gradient time (steepness of salt concentration gradient), flow-rate and column length on resolution in much wider ranges than had been studied before. It was found that two distinct conditions exist that provide high resolution. The first is a condition which has widely been employed in current high-performance IEC, namely, a combination of short gradient time, high flow-rate and comparatively short column. Separation times are usually 5-30 min, and even more rapid (1-2 min) separations are possible. The second is the condition which has rarely been employed in high-performance IEC. It is a combination of long gradient time, low flow-rate and long column. Although it takes several hours for one separation, very high resolution is attainable.

Chromatography, High Pressure Liquid↗

PubMed2003

Batch and simulated moving bed chromatographic resolution of a pharmaceutical racemate.

The preparative chromatographic resolution of racemates has become over the past few years a standard approach for the generation of enantiomers in pharmaceutical research and development. This paper will discuss the chromatographic resolution of a racemic pharmaceutical intermediate. Initial analytical method development to determine the best preparative conditions will be presented. Batch resolution of kg quantities of racemate followed by the simulated moving bed resolution of tens and hundreds of kg of racemate will also be discussed. Finally the different approaches used for the separation will be compared.

Chromatography, Liquid↗

PubMed1998

Liquid chromatographic-high-resolution mass spectrometric and tandem mass spectrometric identification of synthetic peptides using electrospray ionization.

Liquid chromatography-high-resolution electrospray mass spectrometry (LC-ESI-MS) was investigated for the identification of known and unknown synthetic peptides in a research effort designed to evaluate the applicability of this and complementary MS techniques for peptide characterization and identification. The monoisotopic molecular masses of five related peptides with molecular masses between 2000 and 2500 u were acquired with a resolution of 3000 (10% valley). Under narrow and wide mass range magnetic sector scanning conditions monoisotopic molecular mass errors were typically in the 10-20 and 30-40 ppm range, respectively. Tryptic maps were generated for each peptide following LC-ESI-MS analysis and collisionally activated dissociation (CAD) in the ESI interface resulted in the production of characteristic product ions that enabled amino acid sequencing of the tryptic fragments. Unknown identification was demonstrated during analysis of an incomplete synthetic peptide reaction mixture. The synthesis of an 18 amino acid peptide, LTTAVKKVLTTGLPALIS, was not successful. In its place were six unknown peptides that were identified on the basis of monoisotopic molecular mass and amino acid sequence data. The monoisotopic molecular masses of these unknowns were determined to within 10-20 ppm with a resolution of 3500 (10% valley). Amino acid sequences for the six peptides were generated during ESI-MS-MS analysis. Finally two synthetic peptides differing only by the incorporation of a 13C at leucine were analysed with a resolution of 6000 (10% valley) to confirm that the isotopic distributions were consistent with theoretical expectations.

Amino Acid Sequence↗

PubMed1998

Total resolution of 17 DL-amino acids labelled with a fluorescent chiral reagent, R(-)-4-(3-isothiocyanatopyrrolidin-1-y1)-7-(N,N-dimethylaminosulfonyl)- 2,1,3-benzoxadiazole, by high-performance liquid chromatography.

Total resolution of 17 DL-amino acids after derivatization with a fluorescent chiral tagging reagent, 4-(3-isothiocyanatopyrrolidin-1-yl)-7-(N,N-dimethylaminosulfony l)-2,1,3- benzoxadiazole [R(-)-DBD-PyNCS], was studied by reversed-phase liquid chromatography. The reaction of the reagent with amino acids proceeds effectively at 55 degrees C for 20 min in the presence of 1% TEA to produce the corresponding fluorescent diastereomers (excitation at 460 nm, emission at 550 nm). Each pair of the resulting derivatives was efficiently separated with water-acetonitrile containing 1% acetic acid as the mobile phase. Peak resolution was in the range of 0.92 (DL-Arg)-9.8 (DL-Cys). Although mutual separation of some DL-amino acids was possible using the elution solvent, simultaneous resolution of 17 DL-amino acids was difficult with a single chromatographic run, even if some gradient elutions were adopted. Therefore, both gradient and isocratic elution systems were used for total resolution of the DL-amino acids. Thus, 17 DL-amino acids were well resolved by a gradient and an isocratic elution systems. The proposed derivatization and elution methods were applied to the determination of DL-amino acids in yogurt. The results showed that some of the L-amino acids, i.e., Glu, Asp, Ser, Gly, Ala, Thr, Pro, Lys, Phe and Met, were found in the methanol extracts of yogurt. On the other hand, the D-amino acids that were identified in the extracts were D-Glu, D-Asp and D-Ala, and the mean % to each L-amino acid were 11.9% (D-Glu), 27.6% (D-Asp) and 56.7% (D-Ala), respectively.

Amino Acids↗

PubMed1999

Capillary zone electrophoresis of rigid submicron-sized particles in polyacrylamide. Solution selectivity, peak spreading and resolution.

Submicron-sized rigid particles can be separated in a size-dependent fashion by electrophoresis in free solution. Yet it has remained unknown whether the presence of polymers in the solution confers an advantage in size-dependent separation of submicron particles and their resolution. The present study addresses that question, using capillary zone electrophoresis of carboxylate modified polystyrene latex microspheres of 55, 140 and 215 nm radius in solutions of linear polyacrylamide in the M(r) range of 0.4.10(6) to 1.14.10(6). Selectivity of particle separation increases in direct relation to the polymer concentration in the concentration range of 0 to 1% (w/v). Selectivity was found to increase with M(r) of the polymer for the particle sets of 55/140 (nm/nm) and 140/215 (nm/nm) but to decrease with polymer M(r) for the 55/215 (nm/nm) set. Peak spreading is a complex and, in the case of the largest particle, non-monotonic function of polymer concentration, with a minimum at concentrations around the entanglement threshold, c*. Consequently, resolution of the 55/215 and 140/215 (nm/nm) sets also exhibits a maximum around the entanglement threshold while resolution for the 55/140 (nm/nm) set increases with a rise of polymer concentrations above c*. Within the range of optimally resolving polymer concentrations there also occurs a maximum of resolution for all particle sets at a field strength in the range of 150 to 250 V cm-1.

Acrylic Resins↗

PubMed1994

Time-frequency structure of the high-resolution ECG.

This study considers the problem of representing high-resolution ECG (HRECG) signals in the time-frequency plane using spectrotemporal mapping (STM). High-resolution ECG signal components overlap in both time and frequency. The central issue with STM techniques is whether sufficient time-frequency resolution exists to discriminate normal and abnormal QRS signals. The trade-off between signal resolution in time and in frequency must be made without a priori knowledge of the HRECG's time-frequency structure. A simulation experiment was performed to examine the time-frequency distribution of normal, abnormal low-level (late potentials), and bundle branch block components of the QRS. Results suggest that discrimination of these signals with STM is problematic. Signals and noise within the HRECG ensemble can, however, be easily distinguished. This observation forms the basis of a new optimally filtered ensemble averaging technique for signal-to-noise ratio enhancement.

Electrocardiography↗

PubMed1990

Interactions between lambda Int molecules bound to sites in the region of strand exchange are required for efficient Holliday junction resolution.

lambda Site-specific recombination proceeds via two sequential single-strand exchanges that first generate and then resolve a Holliday recombination intermediate. The resolution of artificial Holliday junctions (chi-forms) is well suited to studying the mechanisms involved in reciprocal strand exchange because the linear products of this reaction are stable and easily quantitated. To study the interactions between Int molecules bound at the sites of strand exchange, artificial Holliday junctions containing only the seven base-pair overlap region and the four core-type Int binding sites were used as a model system. In vitro resolution of these structures yields products of both top- and bottom-strand exchange. An abortive product resulting from simultaneous cleavage of the top and bottom strands also occurs at low frequency. Inactivation of one of the four Int binding sites by multiple base substitutions does not significantly affect the efficiency of resolution but has a dramatic effect on the directionality, i.e. the choice of top- or bottom-strand exchange. When any two of the four core-type sites are similarly inactivated, strand exchange is very inefficient and the amount of aberrant cleavage is somewhat greater than for the Holliday junction with four intact Int binding sites. Analysis of the resolution products of Holliday junctions with various combinations of defective Int binding sites leads to the following conclusions: (1) three functional core-type Int binding sites are necessary and sufficient for a strand exchange; (2) the Int molecules that are partners in a strand exchange interact with Int bound to a "cross-core" site that is not directly involved in carrying out the reaction; (3) Int molecules bound to the core-type sites interact in a way that reduces the occurrence of abortive double-strand cleavage events.

Bacteriophage lambda↗

PubMed2002

Spontaneous resolution of vesicoureteral reflux: a 15-year perspective.

PURPOSE: The spontaneous resolution rate of vesicoureteral reflux is helpful for determining the need for surgical intervention and the proper followup schedule in patients on antibiotic prophylaxis. We determined the resolution rate by patient rather than by ureter and analyzed the effects of laterality, gender, age and dysfunctional voiding. MATERIALS AND METHODS: We retrospectively reviewed the records of 179 girls and 35 boys who presented between 1981 and 1984 with urinary tract infection and were diagnosed with primary vesicoureteral reflux. Mean age at presentation was 4.2 years and median followup was 3 years. Of the patients 107 (50%) had bilateral reflux and 60 had dysfunctional voiding. In 146 children (68%) reflux spontaneously resolved during the study. Patients were categorized by the worst grade of reflux, maintained on antibiotic prophylaxis and underwent voiding cystourethrography yearly until reflux resolved. Kaplan-Meier curves were constructed to define the resolution rate. RESULTS: Grades I to III reflux resolved at 13% yearly during the initial 5 years of followup and then at 3.5% yearly during subsequent followup. Grade IV to V reflux resolved at 5% rate yearly. Bilateral reflux resolved more slowly than unilateral reflux and it resolved more rapidly in boys than in girls. Untreated dysfunctional voiding had no effect on overall resolution. CONCLUSIONS: Grades I to III primary vesicoureteral reflux diagnosed after urinary tract infection resolve at identical rates and significantly more rapidly than grades IV to V. Early repair of grade IV to V reflux should be considered after age 18 months.

Adolescent↗

PubMed1990

High resolution ultrasonography and pulsed wave Doppler for detection of corporovenous incompetence in erectile dysfunction.

Cavernosometry and cavernosography have been the primary modalities available for detection and mapping of corporovenous incompetence in patients with erectile dysfunction. These procedures are expensive, time-consuming and associated with some morbidity, prompting us to study a less invasive method, high resolution ultrasonography and pulsed wave Doppler ultrasound. We evaluated 13 patients with nonendocrinological, nonneurological erectile dysfunction by high resolution and Doppler ultrasound for flow in the dorsal and cavernosal veins after intracorporeal papaverine. All patients had a nonrigid response to papaverine and a mean maximum cavernous arterial systolic velocity of greater than 25 cm. per second. The 13 patients were subsequently studied by dynamic cavernosometry and cavernosography, which revealed evidence of venous incompetence (12 with dorsal venous leaks and 11 with cavernous venous leaks). Only 5 of the 12 patients with dorsal venous incompetence had flow detected in the dorsal vein by ultrasound and Doppler studies. High resolution and Doppler ultrasound was unable to detect leakage in the cavernous veins. Among the 2 groups of patients with dorsal venous leaks (those with and without flow detectable by Doppler ultrasound) there was no significant difference in mean cavernous artery diameter or mean cavernous arterial maximum velocity. Similarly, there was no significant difference between the 2 groups in induction, maintenance or initial decompression rates on cavernosometry. We conclude that high resolution and Doppler ultrasound cannot replace dynamic cavernosometry and cavernosography as the diagnostic modality for venous incompetence.

Blood Flow Velocity↗

PubMed1998

Resolution of hormonal markers of ectopic gestation: a randomized trial comparing single-dose intramuscular methotrexate with salpingostomy.

OBJECTIVE: To evaluate resolution of serum hCG and progesterone in patients with ectopic pregnancy receiving single-dose intramuscular (IM) methotrexate as compared with those undergoing laparoscopic salpingostomy. METHODS: In this prospective randomized clinical trial, 75 hemodynamically stable women with a diagnosis of ectopic pregnancy were randomized to treatment with single-dose IM methotrexate (1 mg/kg) or laparoscopic salpingostomy. All women had initial, day 4, and weekly serum hCG and progesterone measurements taken until hCG levels were less than 15 mIU/mL. Methotrexate therapy was repeated if posttreatment day 7 hCG levels did not decrease by 15%, as compared with day 4 levels. Success rate was defined as ectopic resolution without the need for the alternate mode of therapy. RESULTS: Thirty-eight women were randomized to treatment with methotrexate and 37 to laparoscopic salpingostomy. The mean (+/-standard deviation) time required for serum progesterone concentrations to decrease to less than 1.5 ng/mL was significantly less for laparoscopic salpingostomy than for treatment with methotrexate: 7.8+/-1.7 and 17.6+/-2.2 days, respectively (P < .01). Within each treatment group, serum progesterone levels resolved (less than 1.5 ng/mL) more rapidly than did hCG levels (less than 15 mIU/mL) (P < .01). No further treatment was required once serum progesterone levels had decreased to less than 1.5 ng/mL. Success rates were similar in both groups: 94.7% (36 of 38) for methotrexate and 91.4% (33 of 36) for laparoscopic salpingostomy. Mean time required for hCG concentrations to decrease to less than 15 mIU/mL was significantly less for laparoscopic salpingostomy than for methotrexate therapy: 20.2+/-2.7 and 27.2+/-2.3 days, respectively (P < .05). Additional methotrexate injections were required in 15.8% (6 of 38) of women randomized to methotrexate therapy. Initial serum hCG levels for patients receiving additional methotrexate doses were 4830+/-1588 mIU/mL as compared with 2133+/-393 mIU/mL for women receiving only one dose (P = .07). CONCLUSION: Serum progesterone levels of less than 1.5 ng/mL are a good predictor of ectopic pregnancy resolution regardless of treatment, and because its return to normal values occurs more rapidly than that of hCG levels, serum progesterone may be a better marker for predicting successful treatment. Although laparoscopic salpingostomy leads to faster resolution of hormonal markers of ectopic gestation, methotrexate is equally successful for treating small unruptured ectopic pregnancies. Initial hCG levels may be a marker for women requiring additional doses of methotrexate.

Abortifacient Agents, Nonsteroidal↗

PubMed1996

Thoracic versus lumbar epidural anesthesia's effect on pain control and ileus resolution after restorative proctocolectomy.

BACKGROUND: Epidural anesthesia as a perioperative adjunct has been shown to provide superior pain control and has been implicated in more rapid ileus resolution after major abdominal surgery, possibly through a sympatholytic mechanism. Studies suggest that the vertebral level of epidural administration influences these parameters. METHODS: One hundred seventy-nine patients (120 male, 59 female; average age, 36 years) underwent restorative proctocolectomy for ulcerative colitis or familial polyposis between 1989 and 1995. Patients were grouped according to type of anesthesia. Group THO (n = 53) received thoracic (T6 to T10) epidurals. Group LUM (n = 51) received lumbar (L2 to L4) epidurals, and group PCA (n = 75) received patient-controlled intravenous narcotic analgesia. Patients were compared for complications, perioperative risk factors, postoperative pain, and ileus resolution. RESULTS: Epidural narcotics, alone or combined with local anesthetics, were administered for an average of 2 (LUM) to 4 (THO) days without significant complications. Infrequent problems related to the epidural catheters included self-limited headaches or back pain (four) and site infections (two). Epidural failure, as measured by conversion to PCA for inadequate pain control, was not significantly greater for LUM (25%) than THO (23%). Average pain scores, rated daily on a visual analog scale, were significantly higher (indicating more pain) for PCA patients (4.2) during postoperative days 1 through 5 than for LUM (3.5) (p < 0.05) and for THO (2.4) (p < 0.05). Ileus resolution, as determined by stool output and return of bowel sounds, was significantly faster in THO than in LUM or PCA (p < 0.05). Resolution of ileus was not significantly different between PCA and LUM (p > 0.05). CONCLUSIONS: Thoracic epidural analgesia has distinct advantages over both lumbar epidural or traditional patient-controlled analgesia in shortening parameters measuring postoperative ileus and in reducing surgical pain. The procedure is safe and associated with low morbidity. Thoracic epidural anesthesia is also economically justifiable and may prove to impact significantly on future postoperative management by reducing length of hospitalization. Our data and those of others are most striking in these regards for patients with thoracic catheters, indicating the importance of vertebral level in epidural drug administration.

Adolescent↗

PubMed1998

Rapid spontaneous resolution of acute subdural hematoma and HIV related cerebral atrophy: case report.

BACKGROUND: The natural history of a traumatic acute subdural hematoma is usually interrupted by its prompt surgical removal. Rapid spontaneous resolution within 48 hours, although infrequently reported, may be, underestimated and demonstrates a benign course of this condition. To our knowledge, this is the first case of rapid spontaneous resolution of an acute subdural hematoma in a patient with HIV encephalopathy and cerebral atrophy. METHODS AND RESULTS: This 27-year-old man, an intravenous drug user with AIDS-related complex and HIV encephalopathy, suffered an acute subdural hematoma due to head injury in a car accident. The hematoma spontaneously resolved within 12 hours, resulting in a favorable outcome with nonoperative treatment. CONCLUSIONS: AIDS related cerebral atrophy may not only have predisposed the patient to the development of an extracerebral collection, but may have also favorably influenced the spontaneous resolution of the hematoma. The mechanism of the hematoma resolution and the influence of HIV related cerebral atrophy is discussed.

AIDS Dementia Complex↗

PubMed1995

Resolution time of Escherichia coli cystitis is correlated with levels of preinfection antibody to the infecting Escherichia coli strain.

OBJECTIVES: A number of studies in animals have demonstrated that immunization against uropathogenic bacteria can lessen the severity or duration of induced urinary tract infections (UTI). This study examined whether preinfection levels of serum or urinary anti-Escherichia coli antibodies were correlated with length of time needed to resolve an induced E coli cystitis. METHODS: Serum and urine anti-E coli antibody levels in 36 control and 42 vaginally immunized cynomolgus monkeys were measured by enzyme-linked immunosorbent assay. Regression analyses were used to determine correlations between resolution time and preinfection antibody level, and to estimate antibody levels that might be associated with effective resolution of an E coli UTI. RESULTS: Linear regression analysis showed significant correlations between short resolution time and high levels of serum immunoglobulin M (IgM), urinary secretory IgA, and urinary IgG specific for the infecting E coli strain. Serum IgM and urinary IgG anti-E coli levels in monkeys that cleared infections early were significantly higher than in animals with protracted infections. Logistic regression estimated the serum IgM and urinary IgG anti-E coli levels associated with a 50% probability of accelerated clearance to be 3.3 micrograms/mL and 2.7 micrograms/24 hours, respectively. CONCLUSIONS: For this primate model, the observed correlations between short resolution time and pre-existing serum and urinary antibody suggest that antibody-mediated immunity is an important component of host defense against UTI.

Animals↗

PubMed1993

Comparison of reliability indices in conventional and high-pass resolution perimetry.

PURPOSE: The purpose of this study is to compare reliability indices in conventional (Humphrey) and high-pass resolution (Ring) perimetry in healthy subjects followed prospectively at 6-month intervals. METHODS: Of the 146 healthy subjects (mean age, 50.24 years; range, 30-84 years) enrolled in the study, 102 have been tested twice and 71 three times. The authors compared the reliability indices, fixation losses, false-positive rate, and false-negative rate between the two techniques, both cross-sectionally and serially. RESULTS: Fixation losses were slightly higher with high-pass resolution perimetry, whereas false-positive errors were higher with conventional perimetry. False-negative errors were uncommon with either technique. Of 319 fields, 30 (9.4%) conventional and 39 (12.2%) high-pass resolution perimetry fields were unreliable using the current suggested reliability criteria. Nearly all unreliable fields were due to high fixation errors. Using alternative criteria derived from baseline 95th percentile values, unreliable fields were attributed more equally to all three reliability parameters. In subjects tested three times, the reliability indices remained constant. CONCLUSION: The results of this study showed that healthy subjects have comparable reliability indices when tested with conventional and high-pass resolution perimetry.

Adult↗

PubMed1996

Improved resolution in the gel electrophoresis of proteins by a periodically interrupted electric field.

The capability of the commercial gel electrophoresis apparatus with intermittent scanning of fluorescence (HPGE-1000, LabIntelligence) to provide time-dependent zone dispersion allows one to quantitate resolution. Using a model protein separation, that between phycoerythrin and fluorescein-labeled conalbumin, resolution was compared between separations conducted at a constant field strength of 80 V/cm and one conducted in 10-s pulses of the same field strength, interrupted periodically by 120 s in the absence of an electric field. Resolution was improved by a factor of two in the discontinuous application of the electric field compared to that obtained in its continuous application. Similarly, the intermittent application of 80 V/cm for 10 s, followed by 120-s pauses, gave rise to twice the resolution obtained from a continuous application of 7 V/cm.

Computer Graphics↗

PubMed2003

Generating high gray-level resolution monochrome displays with conventional computer graphics cards and color monitors.

Display systems based on conventional computer graphics cards are capable of generating images with about 8-bit luminance resolution. However, most vision experiments require more than 12 bits of luminance resolution. Pelli and Zhang [Spatial Vis. 10 (1997) 443] described a video attenuator for generating high luminance resolution displays on a monochrome monitor, or for driving just the green gun of a color monitor. Here we show how to achieve a white display by adding video amplifiers to duplicate the monochrome signal to drive all three guns of any color monitor. Because of the lack of the availability of high quality monochrome monitors, our method provides an inexpensive way to achieve high-resolution monochromatic displays using conventional, easy-to-get equipment. We describe the design principles, test results, and a few additional functionalities.

Algorithms↗

PubMed1998

Non invasive in vivo anatomical studies of the oscine brain by high resolution MRI microscopy.

We describe in this paper an in vivo Magnetic Resonance Imaging (MRI) procedure that allows one to obtain three-dimensional high quality images of the entire brain of small passerine birds such as the canary with a slice thickness of 58 micron and an image resolution of 78 microns. This imaging procedure was completed in 70 min on anaesthetised birds that later recovered uneventfully and could be reused for subsequent additional imaging. To illustrate the high resolution and anatomical detail that can be achieved, examples of coronal images through the entire hypothalamus are provided in the same sectioning plane as the previously published canary brain atlas. The data set can be used to create sections in any desired plane and the entire data set can be viewed from any point of view in a volume rendered image. This provides a useful tool in understanding the three-dimensional organisation of the brain. Similar procedures can also be applied on fixed brains and might allow an even better anatomical resolution of images because time constrains no longer limit the duration of image acquisition. The non-invasive MRI technique enables to study neuroanatomical features with a high resolution and without killing the animal subjects so that measures can be obtained in a same individual both before and after an experimental treatment.

Animals↗