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PubMed1981

Interactions between drugs and polyvinyl chloride infusion bags.

Forty-six injectable drug products, many of which are administered by i.v. infusion, were studied for loss from aqueous solutions stored in polyvinyl chloride infusion bags for various periods of time. The polyvinyl bags were stored in the dark at room temperature for up to three months. Drugs stored in glass vials served as controls. The solutions were assayed spectrophotometrically at regular intervals. The effects of drug concentration and pH on the loss of drug from solution were studied. Octanol-water partition coefficients were used as a gauge of lipid solubility of the drugs. Five of the drug products-clomethiazole edisylate, diazepam, hydralazine hydrochloride, thiopental sodium, and warfarin sodium-were found to be lost to a substantial extent after one week. For all drugs studied, the effects of the initial concentration on drug loss varied. The amount of drug lost over a given time was a function of the pH of the solution. The main physico-chemical determinants controlling drug sorption appeared to be the extent of ionization and the lipid solubility of the drug. For most of the drugs studied, minimal losses from the aqueous solutions were observed over short periods of storage time. Disappearance was slow and time dependent, indicating a diffusion-controlled sorption process. The losses of clomethiazole edisylate, thiopental sodium, and diazepam may be clinically important.

Drug Packaging↗
PubMed1998

Rumen motility during induced hyper- and hypocalcaemia.

Rumen motility was recorded on an experimental cow by means of telemetric signal transfer from strain gauge force transducers fixed surgically on the peritoneal surface of the rumen wall in the left flank. The normocalcaemic cow was given a standard milk fever treatment with calcium borogluconate (400 ml with 14 mg Ca/ml) intravenously. Transient clinical signs were: decreased rumination, muscle ticks, salivation and a heart rate reduction of 20%. Rectal temperature remained unaltered. Frequency of rumen contractions was reduced up to 40% whereas amplitude of contractions did not deviate from baseline values. Hypocalcaemia was induced in a second experiment by iv infusion of Na2EDTA. At 0.60 mmol/l ionized blood calcium periods of no motility were recorded whereas inactivity of rumen activity was persistent at 0.55 mmol/l ionized blood calcium. The cow went down at 0.45-0.48 mmol/l ionized blood calcium at which point the heart rate was increased by 40%. The high sensitivity of the method employed allowed the conclusion that already at a concentration of ionized blood calcium at 1.0 mmol/l both frequency and amplitude of rumen contractions decreased rapidly although eating behaviour and rumination appeared unaffected during the short term observation periods. Implications of this finding towards health and production in transition cows are discussed.

Animals↗
PubMed2001

Constraining of small-ring cyclic ether triads by stereodefined spiroannulation to an inositol orthoformate platform. Solution- and gas-phase alkali metal binding affinities for three- to five-membered ring structural combinations.

The structural features most conducive to complexation of the alkali metal ions Li(+), Na(+), and K(+) in a series of constrained inositol orthoformate derivatives have been probed in solution, in the solid state, and in the gas phase by electrospray ionization mass spectrometry. The eight spirotricyclic polyethers differ in the size of the rings containing the potentially ligating oxygen atoms. Although the ring sizes have been limited to three to five atoms inclusively, the combinations of oxirane, oxetane, and tetrahydrofuran are rather extensive and consist of many options. The overall trend for lithium ion affinity is [5.5.5] > [ 5.5.4] > [4.4.4] > [5.5.3] > [5.4.3] > [4.4.3] > [1.1.1] > [3.3.1], an ordering that correlates with the differing polarizabilities of the oxygen atoms, ease of alignment of the nonbonded electron pairs, and the overall size of the ligand as gauged by nonbonded O......O distances.

Journal Article↗
PubMed2002

Field testing of particulate matter continuous emission monitors at the DOE Oak Ridge TSCA incinerator. Toxic Substances Control Act.

A field study to evaluate the performance of three commercially available particulate matter (PM) continuous emission monitors (CEMs) was conducted in 1999-2000 at the US Department of Energy (DOE) Toxic Substances Control Act (TSCA) Incinerator. This study offers unique features that are believed to enhance the collective US experience with PM CEMs. The TSCA Incinerator is permitted to treat PCB-contaminated RCRA hazardous low-level radioactive wastes. The air pollution control system utilizes MACT control technology and is comprised of a rapid quench, venturi scrubber, packed bed scrubber, and two ionizing wet scrubbers in series, which create a saturated flue gas that must be conditioned by the CEMs prior to measurement. The incinerator routinely treats a wide variety of wastes including high and low BTU organic liquids, aqueous, and solid wastes. The various possible combinations for treating liquid and solid wastes may present a challenge in establishing a single, acceptable correlation relationship for individual CEMs. The effect of low-level radioactive material present in the waste is a unique site-specific factor not evaluated in previous tests. The three systems chosen for evaluation were two beta gauge devices and a light scattering device. The performance of the CEMs was evaluated using the requirements in draft Environmental Protection Agency (EPA) Performance Specification 11 (PS11) and Procedure 2. The results of Reference Method 5i stack tests for establishing statistical correlations between the reference method data and the CEMs responses are discussed.

Environmental Monitoring↗
PubMed1989

Bromodeoxyuridine uptake in the assessment of hyperthermic therapy for intraocular tumor.

Assessment of uveal melanoma response after many nonenucleation therapies is difficult with current modalities, since tumor regression is usually delayed. The goal of most treatments, including ionizing radiation or radiation and adjunct hyperthermia, is to destroy the reproductive capacity of the tumor. Cell cycling analysis with bromodeoxyuridine, a thymidine analogue only incorporated during DNA synthesis, was a useful indication of tumor control after hyperthermia was used to treat a Greene intraocular melanoma model. Cell cycling decreased from a mean of 16% before therapy to less than 1% in all the successfully treated tumors. Cell cycling changes preceded histologic evidence of cell death. In contrast, tumors that grew after insufficient treatment had increased cell cycling to a mean of 25%. Cell cycling studies with bromodeoxyuridine represent a sensitive gauge of the reproductive integrity of the tumor.

Animals↗
PubMed2006

Neural network-based analysis of thiol proteomics data in identifying potential selenium targets.

Generation of a monomethylated selenium metabolite is critical for the anticancer activity of selenium. Because of its strong nucleophilicity, the metabolite can react directly with protein thiols to cause redox modification. Here, we report a neural network-based analysis to identify potential selenium targets. A reactive thiol specific reagent, BIAM, was used to monitor thiol proteome changes on 2D gel. We constructed a dynamic model and evaluated the relative importance of proteins mediating the cellular responses to selenium. Information from this study will provide new clues to unravel mechanisms of anticancer action of selenium. High impact selenium targets could also serve as biomarkers to gauge the efficacy of selenium chemoprevention.

Antineoplastic Agents↗
PubMed1993

Regression of vascular structural changes and calcium metabolism in patients with essential hypertension after long-term monotherapy with enalapril.

We investigated the effect of one year of enalapril monotherapy on vascular structural changes and calcium metabolism in ten patients with essential hypertension. BP decreased from 169-10/103 +/- 10 mmHg during the placebo period to 138-12/82 +/- 10 mmHg after enalapril therapy. Minimal vascular resistance assessed by the venous occlusion technique with strain-gauge plethysmography was higher in the hypertensive patients than in the normotensive subjects (2.7 +/- 1.2 vs. 1.2 +/- 0.3 mmHg/ml/min per 100 ml tissue, P < 0.01). Although the elevated minimal vascular resistance seen in essential hypertensives decreased to 1.7 +/- 0.5 mmHg/ml/min per 100 ml tissue after enalapril (P < 0.01), it remained higher than that of normotensives (P < 0.05). Cytosolic free calcium ([Ca2+]i) in platelets measured by a Qiun-2 fluorescent indicator was higher in essential hypertensives than in normotensives (189 +/- 38 nM and 138 +/- 14 nM, respectively; P < 0.01). [Ca2+]i of essential hypertensives was reduced to 138 +/- 19 nM after treatment. Plasma renin activity was significantly increased after enalapril. Although plasma ionized calcium concentration did not change, parathyroid hormone was significantly increased after enalapril (from 0.36 +/- 0.22 to 0.58-0.32 ng/ml, P < 0.05). During the placebo period, minimal vascular resistance was correlated with [Ca2+]i (r = 0.62, P < 0.01). There was a close relationship between the changes in minimal vascular resistance and [Ca2+]i (r = 0.78, P < 0.01); however the change in minimal vascular resistance was not associated with changes in BP, catecholamine or parathyroid hormone.(ABSTRACT TRUNCATED AT 250 WORDS)

Adult↗
PubMed1988

Criteria that discriminate between native proteins and incorrectly folded models.

Various theoretical concepts, such as free energy potentials, electrostatic interaction potentials, atomic packing, solvent-exposed surface, and surface charge distribution, were tested for their ability to discriminate between native proteins and misfolded protein models. Misfolded models were constructed by introducing incorrect side chains onto polypeptide backbones: side chains of the alpha-helical hemerythrin were modeled on the beta-sheeted backbone of immunoglobulin VL domain, whereas those of the VL domain were similarly modeled on the hemerythrin backbone. CONGEN, a conformational space sampling program, was used to construct the side chains, in contrast to the previous work, where incorrect side chains were modeled in all trans conformations. Capability of the conformational search procedure to reproduce native conformations was gauged first by rebuilding (the correct) side chains in hemerythrin and the VL domain: constructs with r.m.s. differences from the x-ray side chains 2.2-2.4 A were produced, and many calculated conformations matched the native ones quite well. Incorrectly folded models were then constructed by the same conformational protocol applied to incorrect amino acid sequences. All CONGEN constructs, both correctly and incorrectly folded, were characterized by exceptionally small molecular surfaces and low potential energies. Surface charge density, atomic packing, and Coulomb formula-based electrostatic interactions of the misfolded structures and the correctly folded proteins were similar, and therefore of little interest for diagnosing incorrect folds. The following criteria clearly favored the native structures over the misfolded ones: 1) solvent-exposed side-chain nonpolar surface, 2) number of buried ionizable groups, and 3) empirical free energy functions that incorporate solvent effects.

Computer Simulation↗
PubMed2006

Ab initio optical rotatory dispersion and electronic circular dichroism spectra of (S)-2-chloropropionitrile.

Coupled-cluster and density-functional methods have been used to determine specific rotations and electronic circular dichroism (ECD) rotational strengths for (S)-2-chloropropionitrile. Coupled-cluster specific rotations using both the length- and velocity-gauge representations of the electric-dipole operator, computed with basis sets of triple-zeta quality containing up to 326 functions, compare very well with recently reported gas-phase cavity-ring-down polarimetry data. ECD rotational strengths for the six lowest-lying excited states are found to vary in sign, and the second excited state, which has a larger rotational strength than the first by a factor of 4, was found to yield a much larger contribution (by a factor of 10) to the overall negative specific rotation observed both experimentally and theoretically. However, both valence and Rydberg states appear to make substantial contributions to the total rotation, often of opposite sign from the converged/linear-response result. Furthermore, the sum-over-states approach was found to be inadequate for reproducing the specific rotations derived from the linear-response approach, even when 100 excited states (well beyond the estimated ionization limit) were included in the summation. Density-functional specific rotations using the B3LYP functional with basis sets of quadruple-zeta quality containing up to 588 functions are found to be too large compared to experiment by approximately a factor of 2. This error appears to be related to both the underestimation of the electronic excitation energies, as well as concomitant overestimation of the corresponding ECD rotational strengths. Although earlier studies reported good agreement between density-functional specific rotations and experiment when electric-field-dependent functions were used in conjunction with a double-zeta-quality basis set, the results reported here, which are near the basis-set limit, suggest that this agreement may be fortuitous.

Journal Article↗
PubMed2007

Determination of isopropyl-9H-thioxanthen-9-one in packaged beverages by solid-phase extraction clean-up and liquid chromatography with tandem mass spectrometry detection.

A simple method was developed and validated for the trace determination of 2-isopropylthioxanthone (ITX) in packaged drinks. Samples were extracted from the food matrix using acetonitrile:water (60:40, v/v), and further subjected to clean-up and preconcentration using solid-phase extraction prior to analysis by liquid chromatography-tandem mass spectrometry using multiple reaction monitoring (MRM) mode. The use of 2-isopropyl-[(2)H7]thioxanthen-9-one was incorporated into the method as an internal standard. Excellent 3-day interday precision data (RSD 0.72%, n=10), and intraday precision data (RSD 0.52%, n=10) were obtained on a 0.10 microg/L standard solution. Spiked samples (n=8) were used to gauge the accuracy of the method at the concentration levels of 2.5, 100, and 500 microg/kg in food; recoveries ranged from 97.0 to 103.0%. These excellent validation data suggest the exciting possibility of using this method for the determination of low levels of ITX migrating from printed food packaging materials into beverages with a method quantitation limit of 0.50 microg/kg. For the first time, analysis on a range of milk, juice, tea and yoghurt drinks, as well as their respective food packaging materials were performed for comparative studies on their ITX content.

Beverages↗
PubMed2005

Metabolic activation-related CD147-CD98 complex.

Cell surface CD147 protein promotes production of matrix metalloproteinases and hyaluronan, associates with monocarboxylate transporters and integrins, and is involved in reproductive, neural, inflammatory, and tumor functions. Here we combined covalent cross-linking, mass spectrometric protein identification, and co-immunoprecipitation to show selective CD147 association with three major types of transporters (CD98 heavy chain (CD98hc)-L-type amino acid transporter, ASCT2, and monocarboxylate transporters) as well as a regulator of cell proliferation (epithelial cell adhesion molecule). In the assembly of these multicomponent complexes, CD147 and CD98hc play a central organizing role. RNA interference knock-down experiments established a strong connection between CD147 and CD98hc expression and a strong positive association of CD147 (and CD98hc) with cell proliferation. As the CD147-CD98hc complex and proliferation diminished, AMP-activated protein kinase (a cellular "fuel gauge") became activated, indicating a disturbance of cellular energy metabolism. Our data point to a CD147-CD98 cell surface supercomplex that plays a critical role in energy metabolism, likely by coordinating transport of lactate and amino acids. Furthermore we showed how covalent cross-linking, together with mass spectrometry, can be used to identify closely associated transmembrane proteins. This approach should also be applicable to many other types of transmembrane proteins besides those associated with CD98hc and CD147.

AMP-Activated Protein Kinases↗
PubMed2005

Characterisation of derivatised monomeric and prepolymeric isocyanates by matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry and structural elucidation by tandem mass spectrometry.

Isocyanates are an important class of compounds in occupational hygiene monitoring due mainly to their behaviour as respiratory sensitisers. Here, we demonstrate the application of matrix-assisted laser desorption/ionisation mass spectrometry (MALDI-MS) and MALDI tandem mass spectrometry (MS-MS) to the analysis of derivatised isocyanate monomers and prepolymers. The aim of the work has been to gauge the selectivity obtainable from the direct analysis of isocyanate mixtures without prior separation. Monomeric and prepolymeric isocyanate mixtures were analysed as their 1-(2-methoxyphenyl) piperazine derivatives and the potential of MALDI time-of-flight (ToF)-MS for an NCO monitoring program was assessed. The results obtained demonstrated the possibility of direct mixture analysis by this method. MALDI-MS-MS was used for the elucidation of fragment structures in the prepolymer samples. The developed methodology was then applied to the analysis of swabs from an occupational hygiene monitoring scheme and enabled the identification of the isocyanate species detected.

Air Pollutants, Occupational↗
PubMed2007

Dominance of amyloid precursor protein sequence over host cell secretases in determining beta-amyloid profiles studies of interspecies variation and drug action by internally standardized immunoprecipitation/mass spectrometry.

beta-Amyloid peptides, tentatively regarded as the principal neurotoxins responsible for Alzheimer's Disease, make up a set of products that varies significantly among different biological systems. The full implications of this complexity and its variations have yet to be defined. In this work, Abeta peptide populations were extracted from animal brain tissue or cell-conditioned media, immunoprecipitated with specific antibodies, and analyzed by matrix-assisted laser desorption time-of-flight mass spectrometry. (15)N-Substituted Abeta internal standards were added to gauge variations in the profile of captured peptides. Results from a range of species, including guinea pig, dog, rabbit, and wild-type and transgenic mice, showed that the Abeta peptide population in each system was mainly determined by the species of origin of the amyloid precursor protein (APP) and not by the host tissue or cell line. The same method was used to gauge the effect on the Abeta peptide profile of an inhibitor of gamma-secretase, one of the two proteinases that excises Abeta peptides from the precursor protein with different effects on specific peptides. Overall, the results demonstrate that the species of origin of the APP substrate dictates the outcome of APP processing to a greater extent than the origin of the processing enzymes, an important consideration in rationalizing the properties of different model systems.

Alanine↗
PubMedDate not supplied

Characterization of human tear proteome using multiple proteomic analysis techniques.

Tear proteome profiling may generate useful information for the understanding of the interaction between an eye and its contacting objects, such as a contact lens or a lens implant. This is important for designing improved eye-care devices and maintaining the health of an eye. Proteome profiles of tear fluids may also be used for disease diagnosis and prognosis. However, only a small volume of tear fluid (<5 microL) can be collected in a clinical laboratory under normal operational conditions, which makes proteome profiling a challenge. In this work we apply several proteomic analysis techniques, including gel-based and solution-based approaches with LC-ESI and LC-MALDI MS and MS/MS to gauge the relative merits of producing proteome profiles and to generate as broad a coverage of the tear proteome as possible from this small amount of sample. It is shown that a total of 54 proteins can be confidently identified using less than 5 microL of tear fluid. Of these, 44 proteins can be detected by LC-MALDI MS alone with a consumption of 2 microL of tear fluid. Furthermore, LC-MALDI can be used to determine post-translational modifications (PTMs), such as glycosylation and phosphorylation, without any sample enrichment or treatment. This work represents one of the most extensive proteome profiles (i.e., proteins identified and PTMs characterized) generated from tear fluids using clinically relevant amounts of sample.

Chromatography↗
PubMed2000

Gamma knife radiosurgery as a primary treatment for prolactinomas.

OBJECT: The purpose of this study was to estimate the efficacy of gamma knife radiosurgery (GKS) in controlling tumor growth and endocrinopathy associated with prolactinomas. METHODS: Between 1993 and 1997, 164 of 469 patients with pituitary adenomas treated by GKS harbored prolactinomas. The dose to the tumor margin ranged from 9 to 35 Gy (mean 31.2 Gy), and the visual pathways were exposed to a dose of less than 10 Gy. The mean tumor diameter was 13.4 mm. The mean follow-up time for 128 cases was 33.2 months (range 6-72 months). Tumor control was observed in all but two patients who underwent surgery 18 and 36 months, respectively, after GKS. Clinical cure was achieved in 67 cases. Clinical improvement was noted with a decrease in the hyperprolactinemia after GKS. Nonetheless, in 31 (29%) of 108 patients who were followed for more than 2 years no improvement in serum prolactin levels was demonstrated, although this could be normalized by bromocriptine administration after treatment. Nine infertile women became pregnant 2 to 13 months after GKS and all gave birth to normal children. There was no visual deterioration related to GKS. Five women experienced premature menopause. In these patients there was subtotal disappearance of the tumor and an empty sella developed. CONCLUSIONS: Gamma knife radiosurgery as a primary treatment for prolactinomas can be safe and effective both for controlling tumor growth and for normalization of prolactin hypersecretion. A higher margin dose (> or = 30 Gy) seemed to be associated with a better clinical outcome. Gamma knife radiosurgery may make prolactinomas more sensitive to the bromocriptine.

Humans↗
PubMed2002

Radiosurgery for residual or recurrent nonfunctioning pituitary adenoma.

OBJECT: Nonfunctioning pituitary adenomas comprise approximately 30% of all pituitary tumors. The purpose of this retrospective study is to evaluate the efficacy and role of gamma knife radiosurgery (GKS) in the management of residual or recurrent nonfunctioning pituitary adenomas. METHODS: A review was conducted of the data obtained in 42 patients who underwent adjuvant GKS at the University of Pittsburgh between 1987 and 2001. Prior treatments included transsphenoidal resection, craniotomy and resection, or conventional radiotherapy. Endocrinological, ophthalmological, and radiological responses were evaluated. The duration of follow-up review varied from 6 to 102 months (mean 31.2 months). Fifteen patients were observed for more than 40 months. The mean radiation dose to the tumor margin was 16 Gy. Conformal radiosurgery planning was used to restrict the dose to the optic nerve and chiasm. Tumor control after GKS was achieved in 100% of patients with microadenomas and 97% of patients with macroadenomas. Gamma knife radiosurgery was equally effective in controlling adenomas with cavernous sinus invasion and suprasellar extension. No patient developed a new endocrinological deficiency following GKS. One patient's tumor enlarged with an associated decline in visual function. Another patient experienced a deterioration of visual fields despite a decrease in tumor size. CONCLUSIONS: Gamma knife radiosurgery can achieve tumor control in virtually all residual or recurrent nonfunctioning pituitary adenomas. Dose sparing facilitates tumor management even when the adenoma is close to the optic apparatus or invades the cavernous sinus.

Adenoma↗