orabase and acetonitrile

Water-soluble sampling materials for DBS have been introduced to solve some of the common challenges of DBS.. Carboxymethyl cellulose (CMC) as water-soluble material was evaluated for small proteins using insulin as model analyte. 15 µl of whole blood was deposited and dried on a sheet of CMC prior to dissolvation of the whole spot, matrix precipitation with acetonitrile and LC-MS/MS analysis.. CMC was shown to promote matrix precipitation resulting in cleaner extracts than precipitation without CMC present. The recovery of insulin from the spot was 68 ± 4%, and the spotted samples were stable for at least 1 week in room temperature.. Water-soluble DBS showed promising performance also in analysis of small proteins.

Topics: Acetonitriles; Blood Specimen Collection; Carboxymethylcellulose Sodium; Chemical Precipitation; Chromatography, Liquid; Dried Blood Spot Testing; Humans; Insulin; Limit of Detection; Solubility; Tandem Mass Spectrometry; Water

A rapid, sensitive, specific and selective LC-MS/MS method for the determination of zerumbone (ZER) in human plasma using 2,4-diamino-6-(4-methoxyphenyl)-1,3,5-triazine (DMTZ) as an internal standard (IS) has been developed and validated. ZER was chromatographed on C8 column using a mobile phase of acetonitrile/water (80:20, v/v) at a flow rate of 0.25 ml min(-1) . Quantitation was achieved using ESI+ interface, employing multiple reaction monitoring (MRM) mode at m/z 219 > 81 and 218 > 134 for ZER and IS, respectively. The calibration standards were linear over a range of 5-3000 ng ml(-1) (r(2)=0.9994) with an LLOQ of 5 ng ml(-1) (RSD %; 11.4% and bias%; 9.5%). Intra- and inter-day precision of ZER assay ranged from 0.18 to 3.56% with accuracy (bias) that varied between -5.09 and 4.3%, demonstrating good precision and accuracy. Recoveries of ZER and the IS from human plasma were above 85%. The developed method was validated for the determination of ZER in rat plasma. Linearity, stability of ZER and the ME on rat plasma were discussed. The applicability of the developed method was demonstrated by measuring ZER in rat plasma samples following intravenous and intraperitoneal administration of ZER prepared in hydroxypropyl-β-cyclodextrin (HPβCD) and sodium carboxymethyl cellulose (CMC), respectively, in 20 mg kg(-1) and this study indicated a clear significant difference (p<0.05) in pharmacokinetic parameters of ZER in ZER/HPβCD complex compared with ZER in CMC preparation.

Topics: 2-Hydroxypropyl-beta-cyclodextrin; Acetonitriles; Analysis of Variance; Animals; beta-Cyclodextrins; Carboxymethylcellulose Sodium; Chromatography, Liquid; Drug Stability; Humans; Least-Squares Analysis; Male; Rats; Rats, Sprague-Dawley; Reproducibility of Results; Sensitivity and Specificity; Sesquiterpenes; Spectrometry, Mass, Electrospray Ionization; Tandem Mass Spectrometry

Precise measurements on the electrical conductivity of solutions of sodium salt of carboxymethylcellulose in acetonitrile/water mixed-solvent media containing 10, 20, and 40 vol % of acetonitrile are reported as a function of temperature. The degree of substitution of carboxymethylcellulose used was 0.70, and the concentrations were varied from approximately 1 x 10(-4) to approximately 1 x 10(-2) equiv L(-1). The results showed a decrease in the equivalent conductivity with increasing polyelectrolyte concentration. The applicability of Manning's theory for salt-free polyelectrolyte solutions was examined, and a major discrepancy against the theory was observed. The calculated values of the equivalent conductivity deduced on the basis of this theory were found to be higher than the experimental ones. Possible reasons for this discrepancy have been discussed. The fractions of uncondensed counterions were evaluated, and these were found to depend on the polyelectrolyte concentration. The effects of the temperature and relative permittivity of the medium on the equivalent conductivity as well as on the fraction of uncondensed counterions were also investigated.

Topics: Acetonitriles; Carboxymethylcellulose Sodium; Chemistry, Physical; Electric Conductivity; Electrochemistry; Electrolytes; Ions; Models, Chemical; Polymers; Salts; Static Electricity; Temperature; Water