12 research outputs found
Residual thiosulfate determination in omeprazole by liquid chromatography
An HPLC-UV method for the determination of thiosulfate in aqueous media was modified and validated in this study to quantify the amount of residual thiosulfate in omeprazole samples. Absorption of thiosulfate ion was monitored at 215 nm in alcoholic tetrabutylammonium hydroxide solution as a mobile phase, in which the pH was adjusted to 6.20 by using dilute hydrochloric acid. A method detection limit of 0.08 mg/L was achieved for thiosulfate ion in 1000 mg/L omeprazole solution. The precision, accuracy, and the expanded uncertainty of the method were 2.7 %, 92.4-102.6 %, and 2.2 % (at 95 % confidence level (k = 2) assuming 1.0 mg/L thiosulfate in the sample solution), respectively
Open reduction technique for overlapping and locked pubic symphysis
A locked pubic symphysis can occur following a lateral compression injury of the pelvic ring when one pubic bone becomes entrapped behind the contralateral pubis or obturator foramen, In selecting the treatment modality, it is important to know the mechanism of injury. We presented the use of an open reduction technique in the treatment of a locked pubic symphysis in which open reduction external fixation application failed in the emergency department
Chemical Composition of Natural Colophony from Pinus brutia and Comparison with Synthetic Colophony
The compositions of colophony resins obtained from Pinus brutia Ten trees by three different methods (acid paste, carved hole and scraping) from Ayvacik, Gokova and Kemalpasa in Turkey were analyzed by capillary GC-MS The main components were the monoterpenes alpha-pmene, beta-pinene, and Delta(3) carene, and the diterpenic resin acids palustric, abietic, kaur-9(11)-16-en-18-oic and neoabietic acid The synthetic colophony resins exhibited similar contents to those of the natural resins obtained from the Gokova and Kemalpasa regions of Turkey However, colophony resins from Ayvacik exhibited only half the diterpenic acid content as those of the Gokova and Kemalpasa resins Out of the three techniques, the carved hole method caused rather different percentages in the constituents of the essential oil
Proteomic Analysis of Kidney Preservation Solutions Prior to Renal Transplantation
One of the main issues in kidney transplantation is the optimal functional preservation of the organ until its transplantation into the appropriate recipient. Despite intensive efforts, the functional preservation period remains limited to hours. During this time, as a result of cellular injury, various proteins, peptides, and other molecules are released by the organ into the preservation medium. In this study, we used proteomic techniques to analyze the protein profiles of preservation solutions in which organs had been preserved prior to their transplantation. Samples were obtained from the preservation solutions of 25 deceased donor kidneys scheduled for transplantation. The protein profiles of the solutions were analyzed using 2D gel electrophoresis/MALDI-TOF and LC-MS/MS. We identified and quantified 206 proteins and peptides belonging to 139 different groups. Of these, 111 proteins groups were belonging to kidney tissues. This study used proteomic techniques to analyze the protein profiles of organ preservation solutions. These findings will contribute to the development of improved preservation solutions to effectively protect organs for transplantation
Proteomic Analysis of Liver Preservation Solutions Prior to Liver Transplantation
Objective: Transplantation is the preferred treatment for patients with end-stage liver diseases. However, in clinical practice, functional preservation of the liver is a major concern before the transplantation. Although various protective solutions are used (in combination with hypothermia), the functional preservation time for liver is still limited to hours. We analyzed the preservation medium to detect the proteins released from the liver during storage period
Protein spots of kidney preservation solution identified by 2D gel electrophoresis.
<p>Protein spots of kidney preservation solution identified by 2D gel electrophoresis.</p
List of proteins and peptides that were isolated from kidney preservation solution which showed a statistically significant correlation with donors’ age (DA), cold ischemia time (CIT), creatinine (Cr) and blood urea nitrogen (BUN).
<p>List of proteins and peptides that were isolated from kidney preservation solution which showed a statistically significant correlation with donors’ age (DA), cold ischemia time (CIT), creatinine (Cr) and blood urea nitrogen (BUN).</p
Proteins and peptides belonging to kidney tissues detected from preservation solution using LC-MS/MS (n:18).
<p>Proteins and peptides belonging to kidney tissues detected from preservation solution using LC-MS/MS (n:18).</p
Final report on key comparison CCQM-K55.c (L-(+)-Valine): Characterization of organic substances for chemical purity
Under the auspices of the Organic Analysis Working Group (OAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM) a key comparison, CCQM K55.c, was coordinated by the Bureau International des Poids et Mesures (BIPM) in 2012. Twenty National Measurement Institutes or Designated Institutes and the BIPM participated. Participants were required to assign the mass fraction of valine present as the main component in the comparison sample for CCQM-K55.c. The comparison samples were prepared from analytical grade L-valine purchased from a commercial supplier and used as provided without further treatment or purification.
Valine was selected to be representative of the performance of a laboratory's measurement capability for the purity assignment of organic compounds of low structural complexity [molecular weight range 100–300] and high polarity (pKOW > −2).
The KCRV for the valine content of the material was 992.0 mg/g with a combined standard uncertainty of 0.3 mg/g. The key comparison reference value (KCRV) was assigned by combination of KCRVs assigned from participant results for each orthogonal impurity class. The relative expanded uncertainties reported by laboratories having results consistent with the KCRV ranged from 1 mg/g to 6 mg/g when using mass balance based approaches alone, 2 mg/g to 7 mg/g using quantitative 1H NMR (qNMR) based approaches and from 1 mg/g to 2.5 mg/g when a result obtained by a mass balance method was combined with a separate qNMR result.
The material provided several analytical challenges. In addition to the need to identify and quantify various related amino acid impurities including leucine, isoleucine, alanine and α-amino butyrate, care was required to select appropriate conditions for performing Karl Fischer titration assay for water content to avoid bias due to in situ formation of water by self-condensation under the assay conditions. It also proved to be a challenging compound for purity assignment by qNMR techniques.
There was overall excellent agreement between participants in the identification and the quantification of the total and individual related structure impurities, water content, residual solvent and total non-volatile content of the sample. Appropriate technical justifications were developed to rationalise observed discrepancies in the limited cases where methodology differences led to inconsistent results.
The comparison demonstrated that to perform a qNMR purity assignment the selection of appropriate parameters and an understanding of their potential influence on the assigned value is critical for reliable implementation of the method, particularly when one or more of the peaks to be quantified consist of complex multiplet signals.JRC.D.2-Standards for Innovation and sustainable Developmen