Effect of high pressure on cod (Gadus morhua) desalting

The effect of high pressure on salt and water diffusion in the desalting process of cod was studied. Under pressure, up to 300 MPa, the osmotic equilibrium is reached much faster, compared to desalting at atmospheric pressure. Water (D _ew) and salt (D _es) effective diffusion coefficients reached a maximum at 200 MPa, increasing 500- and 160-fold, respectively, compared with desalting at atmospheric pressure. Increasing pressure up to 300 MPa causes a reduction in both effective diffusion coefficients, although they were still about 70-fold higher than at atmospheric pressure. Up to 200 MPa, a linear correlation was found between D _ew and D _es and pressure. However, the total diffused amounts of water and salt, when the osmotic equilibrium was reached, were lower under pressure. At atmospheric pressure cod water content increased 1.65-fold, but under pressure the increment was on average 1.25-fold, while salt content decreased to 0.51-fold the initial value at atmospheric pressure and to around 0.75-fold under pressure.     

Production of potassium sulfate from potassium hydrosulfate solutions using alcohols

Potassium sulfate is used to produce multicomponent fertilizers, free of chlorides. The desalting out of potassium sulfate from an aqueous solution of potassium hydrosulfate was conducted using 40 mass %, 45 mass %, or 50 mass % aqueous solutions of either methanol or propan-2-ol. Composition of the resultant precipitate was analyzed using chemical methods and XRD analysis. The results of the XRD analysis revealed that the main precipitate phase is K₂SO₄. Small amounts of K₅H₃(SO₄)₄ were detected when the desalting out was carried out from 2.5 M KHSO₄ solution using 40 mass % and 50 mass % methanol solution. When the amount of potassium bisulfate in the solution increased to 3.5 M and 3.8 M, the main phase consisted of K₃H(SO₄)₂. Generally, the desalting out process using propan-2-ol caused the formation of K₃H(SO₄)₂. Potassium sulfate was obtained only by desalting out the 2.5 M KHSO₄ solution using 50 mass % aqueous propan-2-ol. Presented at the 34th International Conference of the Slovak Society of Chemical Engineering, Tatranské Matliare, 21–25 May 2007.     

Online microdialysis-dynamic nanoelectrospray ionization-mass spectrometry for monitoring neuropeptide secretion

Although mass spectrometric approaches offer a sensitive method for identifying cell-cell signaling peptides, the high salt-containing environment of extracellular solutions often complicates characterization of these microscale samples. Accordingly, we have developed a miniature hollow-fiber microdialysis device optimized for desalting small-volume neuronal samples online, with the device directly connected to a modified dynamic nanoelectrospray ionization assembly interfaced with an ion trap mass spectrometer. Improvements over existing designs include placement of a capillary insert within the microdialysis fiber to minimize volume, as well as the use of a microinjector that enables 1 microl sample injections. We present detailed evaluation of peptide recoveries within the microdialysis fiber by liquid chromatography-electrospray ionization-ion trap-mass spectrometry analysis of tissue homogenate in artificial seawater with and without microdialysis. Analyte recoveries after microdialysis ranged from 6 to 78% with higher recoveries of more hydrophilic peptides, while little correlation between mass and percentage recovery was observed in the range studied (2000 to 6000 Da). Recoveries of peptides were the lowest for the analytes with the highest initial mass spectrometry signal intensity. Finally, we illustrate the utility of this microdialysis device for desalting neuropeptides secreted from preparations of the peptidergic bag cell neurons of the marine mollusk, Aplysia californica. Without microdialysis, the high concentration of salts ( approximately 0.5 M) prevented detection of peptides, whereas following online microdialysis-dynamic nanoelectrospray mass spectrometry of stimulated releasate, three peptides (acidic peptide, acidic peptide 1-24 and delta-bag cell peptide) were detected.     

Optimization of reversed-phase solid-phase extraction for shotgun proteomics analysis By Fanni Bugyi,Lilla Turiák,László Drahos and Gábor Tóth

Reversed-phase solid-phase extraction (SPE) is the method of choice for the purification of proteomics samples. Even though the efficacy of SPE methods is sample type-dependent, the manufacturers' protocols are used in most studies. Using an optimized SPE method can lead to a substantial gain in identification and recovery. In this tutorial, we give a brief introduction to the most important parameters influencing SPE performance, and we present a short workflow (16 measurements) for optimizing the SPE procedure. This is complemented by method performance assessment instructions and a short troubleshooting guide to help users further understand and investigate their SPE methods.