Search PubMed⌕ Search

SEARCH · Search PubMed

Results for “TITRATION”

Search indexed PubMed citations on genomics, clinical trials, systematic reviews and public health. Explore titles, authors and supplied subject terms, then open the PubMed record.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 739 records · Page 41Linked to original sources
PubMed2006

Calibration in isothermal titration calorimetry: heat and cell volume from heat of dilution of NaCl(aq).

An isothermal titration calorimeter of the perfusion type (MicroCal model VP-ITC) is calibrated using the heat of dilution of NaCl in water. The relative apparent molar enthalpy function (L(phi)) for NaCl(aq) varies strongly and nonlinearly with concentration in the low-concentration region (<0.2M) that is sampled easily and extensively in a single program of injections of NaCl solution into water. This nonlinearity makes it possible to calibrate with respect to two quantities: the measured heat and the active cell volume. The heat factor is determined with typical standard error 0.003; its value in the current case is 0.987. The cell volume factor is 0.93 but is quite sensitive to possible systematic errors in the temperature and in the literature values for L(phi). Both correction factors are closely tied to the delivered volume from the injection syringe, which required a correction factor of 0.973, attributed to an instrumental gear ratio error. Temperature calibration of the instrument showed a small offset of 0.12K at the temperature 25 degrees C of the experiments, but the error increased to more than 1K at 46 degrees C. The experiments were not able to distinguish clearly between mixing algorithms that assume instantaneous mixing on injection and those that assume instantaneous injection followed by mixing; however, examination of these algorithms has revealed an error in a program widely used to analyze isothermal titration calorimetry data.

Algorithms↗
PubMed2005

Equilibrium titrations of acid-induced unfolding-refolding and salt-induced molten globule of cytochrome c by FT-IR spectroscopy.

Despite extensive investigations on the acid-unfolded and acid/salt-induced molten globule(-like) states of cytochrome c using variety of techniques, structural features of the acid-unfolded state in terms of residual secondary structures and the structural transition between the acid-unfolded and acid/salt-refolded states have not been fully characterized beyond the circular dichroism (CD) spectroscopy. It is unusual that secondary structure(s) of the unfolded state leading to the molten globule state, an important protein folding intermediate, as determined by CD was not fully corroborated by independent experimental method(s). In this study, we carried out an equilibrium titration of acid-induced unfolding and subsequent acid- and salt-induced refolding of cytochrome c using Fourier transform infrared spectroscopy. The spectral profiles of the equilibrium titration reveal new structural details about the acid-unfolded state and the structural transition associated with the acid/salt-refolded molten globule(-like) states of cytochrome c.

Cytochrome c Group↗
PubMed2004

Efficacy of accelerated dose titration of olanzapine with adjunctive lorazepam to treat acute agitation in schizophrenia.

We conducted a prospective double-blind study of accelerated dose titration of olanzapine in the treatment of newly admitted acutely agitated patients with schizophrenia. Patients were randomized to either oral olanzapine (10 mg per day) or oral haloperidol (10 mg per day), plus lorazepam as needed (up to 12 mg per day). Antipsychotic dosage was increased to 20 mg per day as early as day 3. Patients were evaluated with the Positive and Negative Syndrome Scale (PANSS) Agitation subscale during the first 24 hours of treatment, daily for the first week, then weekly until study completion. Significant within-group improvement was demonstrated in PANSS Agitation scores for both groups as early as 1 hour after initiating therapy (-5.79 +/- 6.30 for olanzapine and -4.89 +/- 6.05 for haloperidol, P <.001). This study demonstrated that accelerated dose titration of oral olanzapine is as efficacious as oral haloperidol in reducing acute agitation in patients with schizophrenia.

Acute Disease↗
PubMed2006

Probing the mechanism of purine nucleoside phosphorylase by steady-state kinetic studies and ligand binding characterization determined by fluorimetric titrations.

Reversible reaction catalyzed by trimeric purine nucleoside phosphorylase (PNP) from Cellulomonas sp. with typical and non-typical substrates, including product inhibition patterns of both reaction directions, and interactions of the enzyme with bisubstrate analogue inhibitors, were investigated by the steady-state kinetic methods and fluorimetric titrations. The ligand chromophores exist most probably as neutral species, and not N(1)-H monoanions, in the complex with PNP, as shown by determination of inhibition constants vs. pH. This supports the mechanism in which hydrogen bond interaction of N(1)-H with Glu204 is crucial in the catalytic process. Stoichiometry of ligand binding, with possible exception of hypoxanthine, is three molecules per enzyme trimer. Kinetic experiments show that in principle the Michaelis-Menten model could not properly describe the reaction. However, this model seems to hold for certain experimental conditions. Data presented here are supported by earlier findings obtained by means of fluorimetric titrations and protective effects of ligands on thermal inactivation of the enzyme. All results are consistent with the following mechanism for trimeric PNPs: (i) random binding of substrates, (ii) potent binding and slow release of some reaction products leading to the circumstances that the chemical step is not the slowest one and that rapid-equilibrium assumptions do not hold, (iii) a dual role of phosphate--a substrate and also a reaction modifier.

Catalysis↗
PubMed2005

Establishment of a national network of validated and qualified laboratories for neutralizing anti-vaccinia antibodies titration.

A Proficiency Testing Study (PTS) was organized in France by the French Health Products Safety Agency (Afssaps) aiming at assessing the performance of laboratories in performing a neutralizing anti-vaccinia antibodies titration method by plaque reduction neutralization test (PRNT). The ultimate goal was to establish a national network of qualified and validated laboratories. Five laboratories were included in the PTS and four submitted their data. Three samples of human sera containing various immunoglobulin concentrations (a "high" serum: s-576, a "medium" serum: Ref-19584 and a "low" serum: s-483) were tested by PRNT as described in a procedure supplied by Afssaps and developed in each laboratory during preliminary assays. Data were sent to Afssaps which performed the statistical analysis. The overall performance of the four participating laboratories was satisfactory. This allowed the four participating laboratories to be validated and then to be qualified by the Ministry of Health. Finally a national network for anti-vaccinia immunoglobulins titration was established.

Antibodies, Viral↗
PubMed2004

Isothermal acid-titration calorimetry for evaluating the pH dependence of protein stability.

A new method, which can be called as isothermal acid-titration calorimetry (IATC), was proposed for evaluating the enthalpy of protein molecules as a function of pH using isothermal titration calorimetry (ITC). This measurement was used to analyze the acid-denaturation of bovine ribonuclease A. The enthalpy change by acid-denaturation of this protein was estimated as 310 kJ/mol at pH 2.8 and 40 degrees C. This value agreed well with the enthalpy change obtained by differential scanning calorimetry. The midpoint pH and proton binding-number difference observed by IATC agreed well with those of the acid transition of the three-dimensional structure monitored by circular dichroism spectrometry. The van't Hoff enthalpy of the transition was derived from the temperature dependence of the midpoint pH and the proton binding-number difference. It agreed well with the calorimetric enthalpy change directly observed by IATC, strongly indicating that there was no stable intermediate state during the acid transition of this protein.

Algorithms↗
PubMed2005

Comparison of the helix-coil transition of a titrating polypeptide in aqueous solutions and at the air-water interface.

The transition from alpha-helix to random coil of the titrating polyamino acid co-poly-L-(lysine, phenylalanine), (p-(Lys,Phe)), has been investigated as a function of pH and ionic strength in aqueous solution and at the air-water interface by means of circular dichroism (CD) spectroscopy and the Langmuir surface film balance technique. The results strongly suggest that the helix-coil transition for peptides at the air-water interface can be determined by using the two-dimensional Flory exponent, nu, to express the pH dependent peptide surface conformation. The helix-coil titration curve of p-(Lys,Phe) shifts approximately 2.5 pH units towards lower pH at the air-water interface, as compared with the bulk solution. This finding is of relevance for the understanding of conformation and conformational changes of membrane-transporting and membrane penetrating peptides as well as for the use of peptides in molecular devices.

Air↗
PubMed2006

Limitations of pH-potentiometric titration for the determination of the degree of deacetylation of chitosan.

The degree of deacetylation (DDA) of chitosan determines the biopolymer's physico-chemical properties and technological applications. pH-Potentiometric titration seems to offer a simple and convenient means of determining DDA. However, to obtain accurate pH-potentiometric DDA values, several factors have to be taken into consideration. We found that the moisture content of the air-dry chitosan samples can be as high as 15%, and a reasonable fraction of this humidity cannot be removed by ordinary drying. Corrections have to be made for the ash content, as in some samples it can be as high as 1% by weight. The method of equivalence point determination was also found to cause systematic variations in the results and in some samples extra acid as high as 1 mol% of the free amino content was also identified. To compensate for the latter effect, the second equivalence point of the titration has to be determined separately and the analytical concentration of the acid be corrected for it. All the corrections listed here are necessary to obtain DDA values that are in reasonable agreement with those obtained from (1)H NMR and IR spectroscopic measurements. The need for these corrections severely limits the usefulness of pH-metry for determining accurate DDA values and thus potentiometry is hardly able to compete with other standard spectroscopic procedures, that is, (1)H NMR spectroscopy.

Acetylation↗
PubMed2004

Feed-forward dose control of wastewater chlorination using on-line pH and ORP titration.

In this study, a simple automatic pH-ORP titration device was developed for identifying the various ammonia concentrations and chlorine dose requirements for wastewater chlorination by identifying the peaks in the ORP-slope profiles and knees/valleys in the pH profiles. In addition, breakpoint chlorination experiments have shown that the ORP values at the monochloramine humps and breakpoints are linearly correlated with the ammonia concentrations. Therefore, a feed-forward control strategy, based on the chlorine/ammonia weight ratio (Cl/N), is proposed in this paper, to control the chlorine doses for a continuous wastewater chlorination experiment in a laboratory-scale reactor. The result of this continuous wastewater chlorination experiment has shown that the pH-ORP titration was able to precisely determine the variations of ammonia concentrations in the chlorination influent. Under this control strategy, effective and stable disinfection efficiencies in terms of total coliform count were obtained.

Ammonia↗
PubMed2004

Combination therapy with rosiglitazone and glibenclamide compared with upward titration of glibenclamide alone in patients with type 2 diabetes mellitus.

AIM: To compare the efficacy of combination therapy using rosiglitazone (8 mg per day) and glibenclamide (7.5 mg per day) with upward titration of glibenclamide as monotherapy (maximum dose=15 mg per day) in reducing HbA(1c) levels over 26 weeks in patients with type 2 diabetes mellitus (T2DM). METHODS: Three hundred and forty patients with T2DM inadequately controlled (FPG > or =7.0 and < or =15.0 mmol/l) on glibenclamide 7.5 mg per day were randomised to either additional treatment with rosiglitazone 8 mg per day or up-titration of the glibenclamide dose (maximum dose=15 mg per day). RESULTS: After 26 weeks, treatment with rosiglitazone combination reduced HbA(1c) by 0.81% (P<0.0001) and FPG by 2.4 mmol/l (P<0.0001) compared with glibenclamide monotherapy. HOMA-S and HOMA-B increased by 12 and 28%, respectively (P<0.0001 for both) with combination compared with glibenclamide monotherapy. With rosiglitazone combination and glibenclamide monotherapy, total cholesterol: HDL ratio reduced by 5 and 13%, triglycerides reduced by 6 and 2%, and FFAs reduced by 15 and 8%, respectively. Both treatments were well tolerated and had predictable safety profiles. CONCLUSION: For patients inadequately controlled on glibenclamide, addition of rosiglitazone provides significantly improved glycaemic control compared with uptitration of glibenclamide. This may be preferable to continued monotherapy with higher doses of glibenclamide.

Adult↗
PubMed2005

Success of a multidisciplinary heart failure clinic for initiation and up-titration of key therapeutic agents.

BACKGROUND: Heart failure has a poor prognosis, yet drugs known to improve outcomes are either not prescribed, or prescribed at sub-therapeutic doses. The National Service Framework (NSF) for coronary heart disease recommended specialist heart failure clinics to address this problem but their efficacy has not been evaluated. OBJECTIVES: To determine the effectiveness of a protocol-driven heart failure clinic staffed by nurse and pharmacist specialists for improving symptoms and optimising treatment with key therapeutic agents, without adversely affecting renal function. RESULTS: Of the 234 patients with at least one follow-up visit, 127 (57%) were receiving none or only one key therapeutic agent when first seen, this was reduced to 25 patients (11%) at most recent follow-up. The improvement in prescription rates was accompanied by significant up-titration of dose, the proportion of patients on "medium" or "high" doses rising from 43 (18%) to 134 (57%) for beta-blockers, and from 129 (55%) to 201 (86%) for ACE-inhibitors/angiotensin receptor blockers. Clinical improvement was reflected in reductions in patients with NYHA functional classes III and IV (93 (40%) to 53 (23%)), and in patients with moderate or severe symptoms. Significant reductions in alcohol consumption and cigarette smoking were recorded. Up-titration of treatment was associated with reductions in heart rate and systolic blood pressure; increases in serum potassium and creatinine concentrations were small. CONCLUSION: In a heart failure clinic staffed by nurse and pharmacist specialists, it is possible to achieve target doses of key therapeutic agents and improve symptoms without adversely affecting electrolytes or renal function.

Adrenergic beta-Antagonists↗
PubMed2004

Features of the ESI mechanism that affect the observation of multiply charged noncovalent protein complexes and the determination of the association constant by the titration method.

Several factors, attributable to the ESIMS mechanism, that can affect the assumptions of the titration method are examined: (1) The assumption that the concentrations in solution of the protein P, the ligand L, and the complex PL are proportional to the respective ion intensities observed with ESIMS, is examined with experiments in which ion intensities of two non-interacting proteins are compared with the respective concentrations. The intensities are found to be approximately proportional to the concentrations. The proportionality factors are found to increase as the mass of the protein is decreased. Very small proteins have much higher intensities. The results suggest that it is preferable to use only the intensity ratio of PL and P, whose masses are very close to each other when L is small, to determine the association constant KA in solution. (2) From the charge residue model (CRM) one expects that the solution will experience a very large increase of concentration due to evaporation of the precursor droplets, before the proteins P and PL are produced in the gas phase. This can shift the equilibrium in the droplets: P + L = PL, towards PL. Analysis of the droplet evaporation history shows that such a shift is not likely, because the time of droplet evolution is very short, only several micros, and the equilibrium relaxation time is much longer. (3) The droplet history shows that unreacted P and L can be often present together in the same droplet. On complete evaporation of such droplets L will land on P leading to PL and this effect will lead to values of KA that are too high. However, it is argued that mostly accidental, weakly bonded, complexes will form and these will dissociate in the clean up stages (heated transfer capillary and CAD region). Thus only very small errors are expected due to this cause. (4) Some PL complexes may have bonding that is too weak in the gas phase even though they have KA values in solution that predict high solution PL yields. In this case the PL complexes may decompose in the clean up stages and not be observed with sufficient intensity in the mass spectrum. This will lead to KA values that are too low. The effect is expected for complexes that involve significant hydrophobic interaction that leads to high stability of the complex in solution but low stability in the gas phase. The titration method is not suited for such systems.

Multiprotein Complexes↗
PubMed2005

Cell surface groups of two picocyanobacteria strains studied by zeta potential investigations, potentiometric titration, and infrared spectroscopy.

In order to clarify the role of picocyanobacteria in aquatic biogeochemical processes (e.g., calcite precipitation), cell surface properties need to be investigated. An experimental study of the cell surface characteristics of two Synechococcus-type unicellular autotrophic picocyanobacterial strains was carried out. One strain was isolated from Lake Plon and contained phycocyanin, the other strain came from Lago Maggiore and was rich in phycoerythrin. Potentiometric titrations were conducted to determine the different types of sites present on the bacteria cell walls. Infrared spectroscopy allowed characterization of the various functional groups (RNH(2), RCOOH, ROH, RPO(2)) and investigations of zeta potential provided insight into the isoelectrical points of the strains. Titrations reveal three distinct sites on the bacterial surfaces of phycocyanin- and phycoerythrin-rich strains with pK values of 4.8+/-0.3/5.0+/-0.2, 6.6+/-0.2/6.7+/-0.4, and 8.8+/-0.1/8.7+/-0.2, corresponding to carboxyl, phosphate, and amine groups with surface densities of 2.6+/-0.4/7.4+/-1.6 x 10(-4), 1.9+/-0.5/4.4+/-0.8 x 10(-4), and 2.5+/-0.4/4.8+/-0.7 x 10(-4) mol/g of dry bacteria. The deprotonation constants are similar to those of bacterial strains and site densities are also within an order of magnitude of other strains. The phycoerythrin-rich strain had a higher number of binding sites than the phycocyanin-rich strain. The results showed that picocyanobacteria may adsorb either calcium cations or carbonate anions and therefore strongly influence the biogeochemical cycling of calcite in pelagic systems.

Cell Wall↗
PubMed2005

Hydrogen ion titration of alkyldimethylamine oxides by 13C and 1H NMR and conventional methods.

In the hydrogen ion titration of micelles, the degree of ionization of the micelle at a given pH has to be evaluated to obtain a pKa value of micelles (Ka being the proton dissociation constant) at the pH. We compared the degree of ionization obtained from 13C and 1H NMR spectra with that obtained from the stoichiometric method. We used dodecyldimethylamine oxide (C12DMAO) and hexyldimethylamine oxide (C6DMAO) to examine the titration behavior of micelles and monomers, respectively. We determined pKa values of amine oxides both in H2O and D2O. As to the monomer (C6DMAO), the degree of ionization from NMR, alpha(NMR), coincided with that from the conventional stoichiometric method alpha. The difference of pK1 of amine oxide monomer between D2O and H2O was about 0.5: pK1(D) approximately pK1(H) + 0.5. The difference was about the same as that for carboxylic acids. As to the C12DMAO micelle, alphaNMR did not coincide with alpha over a considerable range of alpha. The NMR chemical shift might be influenced by micellar structure changes induced by the ionization, such as the sphere-to-rod transition. The intrinsic logarithmic dissociation constants of the micelle were 5.9+/-0.1 for H2O, and 6.5+/-0.1 for D2O.

Carbon Isotopes↗
PubMed2005

Rapid and reproducible infectivity end-point titration of virulent phage in a microplate system.

The standard method for measuring the number of infectious phages in solution has traditionally been the plaque forming assay. An alternative method is described where the number of lytic, infectious phages is determined in an endpoint titration assay adapted for a microplate system. In this model system, susceptible Escherichia coli B6 at a density of 4 x 10(7) cells/ml, were mixed with an equal volume (100 microl) of PhiX174 diluted serially in a microtest plate. After 3h of incubation on a microplate shaker the endpoint was determined spectrophotometrically and calculated according to the method of Reed and Muench. A well was considered positive for infection if the OD630-value was < or = 10% compared to the OD630-value of the negative control of uninfected cells. ID50-titers were 2.5x higher than the PFU-titers (CV 15%) and the intra assay reproducibility revealed a CV of 9%. The method has several advantages as compared with the conventional PFU-titration. It is less time and material consuming with the possibility to assess several samples at the same time.

Bacteriophage phi X 174↗
PubMed2006

Detection and titration of bluetongue virus in Culicoides insect cell culture by an antigen-capture enzyme-linked immunosorbent assay.

Bluetongue virus (BTV) infects sheep, cattle and other ruminants and is transmitted by Culicoides spp. of biting midges. Virus is typically isolated and characterized by infection of susceptible vertebrate cells that undergo detectable and measurable cytopathic effects. Cell lines derived from C. sonorensis may be useful for virus isolation and studies to better understand BTV replication in the insect vector. However, their use is hampered because BTV infection does not produce significant cytopathic effects in these insect cell cultures. Detection of virus replication in these cells typically requires co-cultivation with susceptible vertebrate cell culture. This report describes the use of an antigen-capture enzyme-linked immunosorbent assay (Ag-Cap ELISA) for direct detection and titration of BTV in cultures of a Culicoides cell line. This assay should facilitate use of this cell line for virus isolation, titration and studies of BTV replication.

Animals↗
PubMed2005

A stable isotope titration method to determine the contribution of acetate disproportionation and carbon dioxide reduction to methanogenesis.

A novel stable isotope titration approach was developed to determine the contributions to total methane production made by CO(2) reduction and the disproportionation of acetate in anoxic environments. (13)CH(4), (12)CH(4), (13)CO(2) and (12)CO(2) production rates were measured in the head space of replicate anaerobic microcosms titrated with increasing amounts of (13)C-labelled substrates. The contribution of CO(2) reduction was calculated from the linear relationship between ratios of labelled and total CH(4) production and ratios of labelled and total CO(2) after the addition of (13)C-bicarbonate. In the case of acetoclastic methanogenesis rates of (13)CH(4) and (12)CH(4) production were fitted to a model based on an assumption that the relationship between the concentration of (13)C-labelled acetate and the rates of labelled and unlabelled methane production followed Michaelis-Menten kinetics. A comparison of the raw data with the model supported the assumption and provided both an estimate of the contribution of acetate to methane production and an estimate of the size of the indigenous acetate pool without the need to measure acetate directly. The method was applied to a freshwater sediment in the English Lake District where it was found that 66.3% (se 4.9) of methane production was due to acetate disproportionation and 28.9% (se 1.9) of methane production resulted from CO(2) reduction. This is in agreement with theoretical predictions and other empirical measurements of methanogenesis.

Acetates↗
PubMed2004

Development of a monoclonal antibody based competitive-ELISA for detection and titration of antibodies to peste des petits ruminants (PPR) virus.

Peste des petits ruminants (PPR) is an acute febrile, viral, disease of small ruminants with great economic importance. A competitive-ELISA (c-ELISA) test was developed for detection of antibodies to PPR virus in the sera samples of goats and sheep. The test uses monoclonal antibody to a neutralizing epitope of haemagglutinin protein of the virus. Based on the distribution of known negative sera samples (n=933) in respect of PPR virus antibodies in the test, a cut-off value was set as 38%. This value was the result of mean of negative population added with two times the standard deviations. A total of 1668 sera samples from goat and sheep and 32 sera from cattle were screened by c-ELISA and virus neutralization test (VNT). Efficacy of c-ELISA compared very well with VNT having high relative specificity (98.4%) and sensitivity (92.4%). The sensitivity of c-ELISA for PPR sero-surveillance could further be increased (95.4%), if the target population is non-vaccinated. c-ELISA test correlated well with VNT (r=0.845) for end-point titration of PPR virus antibody in 64 goat sera samples. It could clearly separate infected population from uninfected in field sera. Using c-ELISA test paired sera samples from 13 goats provided a clear diagnosis of PPR virus infection. Furthermore, antibodies to PPR virus could be successfully detected during 1 year after vaccination in four goats inoculated with an experimental PPR vaccine. Findings suggest that the c-ELISA test developed can easily replace VNT for sero-surveillance, sero-monitoring, diagnosis from paired sera samples and end-point titration of PPR virus antibodies.

Animals↗