Biomedical subjects
Publications and source records attributed to J T Stewart.
A 78-year-old man with a long history of major depression responded well to a course of ECT but relapsed before maintenance treatments could be started. Addition of lithium carbonate resulted in a sustained remission with maintenance treatments. The combination of maintenance ECT and lithium may be safe and effective in selected cases of refractory depression.
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Direct serum injection methods are described for the HPLC determination of selected non-steroidal anti-inflammatory drugs (NSAIDS) on restricted access media (RAM) columns, using either a Pinkerton (ISRP) or semi-permeable surface (SPS) column. Twenty microlitres of a filtered serum sample was injected directly onto each column. Calibration curves were prepared for ketoprofen (1-20 micrograms/mL), fenbufen (0.8-20 micrograms/mL), sulindac (0.8-20 micrograms/mL) and probenecid (1.5-40 micrograms/mL) on the SPS column, and nabumetone (1.5-40 micrograms/mL) and indomethacin (1.5-40 micrograms/mL) on the Pinkerton column. The percentage error and imprecision of the methods were found to be less than 10%. The inter- and intra-day variability for analytes were in the range of 0.15-10%. The limits of quantitation and detection were in the range of 800-1500 and 300-800 ng/mL, respectively, for the analytes studied. A hydrophobic shielded phase (Hisep) column was also investigated and was found to be generally too retentive (> 29 min) for assay of these analytes.
High performance capillary electrophoresis (HPCE) methods are described that will separate the enantiomers of various lobeline analogs synthesized in these laboratories. "Cyclodextrin array analysis" was used for preliminary screening and electrophoresis conditions were optimized for each investigated analog. The lobeline analogs under consideration were investigated as potential nicotinic agonists for the treatment of neurodegenerative disorders, such as Alzheimer's disease. Native alpha (alpha)-, beta (beta)-, and gamma (gamma)-cyclodextrins, methyl-beta-cyclodextrin (M-beta-CD), heptakis-(2,6-di-O-methyl)-beta-cyclodextrin (DM-beta-CD), and heptakis-(2,3,6-tri-O-methyl)-beta-cyclodextrin (TM-beta-CD), hydroxypropyl-alpha-cyclodextrin (HP-alpha-CD), hydroxypropyl-beta-cyclodextrin (HP-beta-CD) and hydroxypropl-gamma-cyclodextrin (HP-gamma-CD) were used as run buffer additives and their effect on the enantiomeric resolution of the lobeline analogs was investigated. The effect of pH, buffer concentration, voltage, temperature and organic modifier concentration on the enantiomeric resolution of the lobeline analogs was investigated. The most suitable conditions for each compound were chosen and, with detection at a wavelength of 200 nm, optimized.
We aimed to determine the effects of simulated stent side-branch dilatation and subsequent redilatation of the central lumen. Following coronary stent implantation it may be necessary to dilate through the side of a stent to maintain branch patency. Branch dilatation through the side of 3.5-mm-diameter stents (AVE GFX, beStent, Crown, MultiLink, and NIR) was simulated in a plexiglass phantom using 2.5-, 3.0-, 3.5-, and 4.0-mm balloons. In further experiments, the main lumen was redilated with a 3.5-mm balloon after 3.0-mm side-branch dilatation. Thereafter, a 3.5-mm central and a 3.0-mm side-branch balloon were simultaneously inflated ("kissing balloons"). The larger the balloon size used for side-branch dilatation, the greater the distortion of the stent immediately distal to the side-branch, which for a 4.0-mm balloon ranged from 36% +/- 2% (Crown) to 65% +/- 6% (NIR). Central lumen redilatation or kissing balloons abolished this stenosis with little reduction of the side-lumen diameter. The main stent lumen compromise caused by side-branch dilatation can be abolished by main-lumen redilatation or by kissing balloons.
Procedural and 1-month outcome data following implantation of the V-Flex Plus stent in our first 54 consecutive patients (35 male; mean age, 62 years) are described. Sixty-four stents were implanted for 60 mainly complex lesions; 48% were left anterior descending; 20%, circumflex; 27%, right coronary artery; and 5%, saphenous vein graft. The Indication for stenting was elective in half of the patients and for a suboptimal result or as a bailout procedure in the other half. The stents were deployed at a mean of 12 atm (range, 6-18) and postdilatated to a mean of 15 atm (range, 8-20). Pre- and postdilatation balloon sizes were 2.96 +/- 0.57 mm and 3.16 +/- 0.34 mm, respectively. The procedural success rate was 98%. There were no deaths or Q-wave myocardial infarctions. One patient suffered a non-Q-wave myocardial infarction and another developed a femoral false aneurysm. At 1-month follow-up, there were no additional events, in particular no revascularization procedures. Eighty-nine percent of patients were free of angina. Implantation of the V-Flex Plus stent is safe and effective with an excellent early success rate comparable to that of published randomized trials and registries of carefully selected patients.
Solution conformations of the polypeptides beta endorphin (beta-END) and a cysteine peptide (CYSP) were investigated with the use of particle beam LC/FT-IR spectrometry. Gradient elution HPLC with mobile phases that contained acetonitrile with 0.1% TFA (v/v) and 0.1% aqueous TFA (v/v) were used. The conformations of both polypeptides were studied in 0.9% sodium chloride injection USP, 5% dextrose in water injection USP and sterile water for injection USP. Additional conformational studies over a pH range of 2-10, temperatures of 25, 50, 75 and 100 degrees C and after storage for 24 h were investigated. The studies indicated that the two polypeptides did not behave similarly under identical conditions. It was observed that both beta-END and CYSP had slightly different conformations in the various parenteral solutions. It was also shown that the conformation of CYSP changed with both pH and temperature while beta-END was conformationally stable to both temperature and pH. The identity of the peptides and the conformationally sensitive charge-state intensities of the peptides were investigated with electrospray ionization mass spectrometry (ESI/MS). The combination of IR and MS data allowed an estimation of solution effects on the conformations of the model polypeptides.
A capillary electrophoresis method was developed to separate and quantitate ephedrine (ED), theophylline (TP) and phenobarbital (PB) in a tablet dosage form. Tablets were ground and extracted with methanol using ultrasonication. Aliquots of standard stock solution were hydrodynamically injected for 5 s at the anodic end. Separation was performed on a fused silica capillary (72 cm x 50 microm i.d.; 50 cm to detector) at an applied voltage of 20 kV with a phosphate run buffer (pH 8.0, 50 mM). Analysis was performed at ambient temperature (23+/-1 degrees C) and the total run time was 9 min with detection at 220 nm. Calibration curves were prepared for ED, TP and PB with methyl p-hydroxy benzoate as internal standard. For each analyte, the correlation coefficients were >0.999 (n = 4). The RSD% of ten replicate injections for each analyte were <1%. The method was applied to the quantitation of ED, TP and PB in a commercial tablet dosage form.
Resistiveness to physical care among patients with dementia is a common and burdensome problem. Forty-nine nursing home residents with dementia were administered the Mini-Mental State Exam (MMSE) and the Royall Executive Interview (EXIT), a specific test of frontal-subcortical function. Nurses rated resistiveness on every shift for 3 days. Correlation with resistiveness ratings was stronger for the EXIT (r=0. 73) than for the MMSE (r=-0. 46); logistic modeling found the EXIT to be a strong independent predictor of resistiveness. Executive dysfunction as measured by the EXIT is a major determinant of resistiveness to care in long-term care residents with dementia, possibly as a result of such patients' tendency toward inertia.
The stability and compatibility of ondansetron hydrochloride with neostigmine methylsulfate, naloxone hydrochloride, midazolam hydrochloride, fentanyl citrate, alfentanil hydrochloride, atropine sulfate, morphine sulfate, meperidine hydrochloride, propofol, droperidol, metoclopramide monohydrochloride, and glycopyrrolate were studied. Ondansetron 1.33 or 1.0 mg/mL was combined with 0.9% sodium chloride injection and each of the 12 drugs in duplicate in plastic syringes (or glass for propofol). The syringes were stored at 21.8-23.4 or 4 degrees C in the dark, except for those containing propofol, which were stored at ambient temperature. Samples were removed at 0, 4, 8, and 24 hours for analysis by high-performance liquid chromatography and pH measurement; the propofol-containing samples were removed at 0, 1, 2, and 4 hours. Syringes were visually assessed for color and clarity, and particulate content was measured with a particle counter at the end of the study period. All solutions containing ondansetron retained more than 90% of their initial ondansetron concentration. Solutions containing each of the other drugs except droperidol retained more than 90% of their initial concentration of these drugs. The solutions containing droperidol retained more than 90% of their initial droperidol concentration for up to eight hours at ambient temperature but precipitated quickly at 4 degrees C. In combinations of ondansetron 1.33 or 1.0 mg/mL and 10 of 12 drugs, all drugs were stable for 24 hours in plastic syringes at 23 and 4 degrees C; ondansetron hydrochloride 1.0 mg/mL and propofol 1.0 and 5.0 mg/mL in admixtures were stable for 4 hours, and droperidol on its own and combined with ondansetron 1.0 mg/mL was stable for no more than 8 hours at ambient temperature.
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Four commonly used barbiturates (phenobarbital, butalbital, pentobarbital and thiopental) were analyzed in human serum using supercritical fluid extraction (SFE) and negative ionization LC/ESI-MS/MS. Barbital was used as the internal standard. Carbon dioxide SFE was performed at 40 degrees C and 500 atm, with a total extraction time of 35 min. The analytes were collected off-line in a liquid trap containing absolute methanol. Samples were then concentrated by vacuum centrifugation. The high performance liquid chromatography separation utilized gradient elution with a total analysis time of 21 min. The precursor and major product ions for the four barbiturates were monitored on a triple quadrupole mass spectrometer with negative ion electrospray ionization (ESI) in the multiple reaction monitoring mode as follows: (1) thiopental (m/z 241.20-->58.00), (2) phenobarbital (m/z 231.10-->188.0), (3) pentobarbital (m/z 225.10-->181.90) and (4) butalbital (m/z 222.80-->179.90). In the case of phenobarbital, pentobarbital and butalbital, the most abundant product ion arises from the loss of 43 u (HCNO loss). However, in the case of thiopental, the most abundant product ion was observed at m/z 58.0 (the [M-183]-ion, or NCS-). Mechanisms for the formation of the collision induced dissociation reaction products of these barbiturates are proposed.
Solution conformations of the peptides angiotensin I (Ang I) and POMC-X (an octapeptide fragment of proopiomelanocortin) were investigated with the use of particle beam liquid chromatography/Fourier transform infrared (LC/FT-IR) spectrometry. Gradient elution high-performance liquid chromatography (HPLC) with mobile phases that contain acetonitrile, 2-propanol, 0.1% heptafluorobutyric acid (HFBA) and 0.1% trifluoroacetic acid (TFA) were used. The conformations of both peptides were studied in 0.9% sodium chloride injection USP, 5% dextrose in water injection USP and sterile water for injection USP. Additional conformational studies over a pH range of 2-10, to a temperature of 75 degrees C and after a storage time of 24 h were investigated. The studies indicated that the two peptides do not behave similarly under identical conditions. It was observed that both Ang I and POMC-X had slightly different conformations in the various parenteral solutions. It was also shown that the conformation of Ang I changed with both pH and temperature while POMC-X was conformationally stable to both temperature and pH. The identity of the peptides and the conformationally sensitive charge-state intensities of the peptides were investigated with electrospray ionization mass spectrometry (ESI/MS). The combination of infrared and mass spectrometric data allowed a thorough estimation of solution effects on the conformations of the model peptides.
A sensitive and stereospecific high-performance liquid chromatography (HPLC) method for the quantitation of ketoprofen enantiomers in human serum was developed. The assay involves the use of an octadecylsilane solid-phase extraction for serum sample clean-up prior to HPLC analysis. Chromatographic resolution of the ketoprofen enantiomers was performed on a nonporous octyldecylsilane column with hydroxypropyl beta-cyclodextrin as the mobile phase additive. The composition of the mobile phase was 98:2 v/v aqueous 0.1% trifluoroacetic acid (TFA), pH 4.00 (adjusted with triethylamine (TEA))/acetonitrile containing 10 mM hydroxypropyl beta-cyclodextrin (beta-CD) at a flow rate of 0.8 ml min-1. Recoveries of R(-)-ketoprofen was 95.4 +/- 2.16% and for S(+)-ketoprofen 96.2 +/- 1.31%. Linear calibration curves were obtained in the range 0.025-15 micrograms ml-1 range for each enantiomer in serum. The detection limit based on a S/N = 3 ratio was 10 ng ml-1 for each enantiomer in serum with ultraviolet detection at 220 nm. The limit of quantitation for each enantiomer was 25 ng ml-1. Precision calculated as % relative standard deviation (%R.S.D.) and accuracy calculated as % error were in the range 0.2-5.2% and 0.3-2.2%, respectively, for the R enantiomer and 0.3-6.2 and 0.2-3.2%, respectively, for the S enantiomer.