Evaluation of fritless solid-phase extraction coupled on-line with capillary electrophoresis-mass spectrometry for the analysis of opioid peptides in cerebrospinal fluid.

Fritless SPE on-line coupled to CE with UV and MS detection (SPE-CE-UV and SPE-CE-MS) was evaluated for the analysis of opioid peptides. A microcartridge of 150 μm id was packed with a C18 sorbent (particle size > 50 μm), which was retained between a short inlet capillary and a separation capillary (50 μm id). Several experimental parameters were optimized by SPE-CE-UV using solutions of dynorphin A (DynA), endomorphin 1 (End1), and methionine-enkephaline (Met).

Optimization of in-line fritless solid-phase extraction for capillary electrophoresis-mass spectrometry.

In this study, in-line frit-free solid-phase extraction (SPE) has been studied for the preconcentration of analytes prior to analysis by capillary electrophoresis-mass spectrometry (CE-MS). The mixed-mode sorbent Oasis HLB was selected for the trapping of compounds of different polarity. Using 2-ethylidene-1,5-dimethyl-3,3-diphenylpirrolidine (EDDP), dihydrocodeine and codeine as test compounds, SPE parameters such as the pH of the sample and composition of the washing and elution solvent were optimized.

Determination of oversulfated chondroitin sulfate and dermatan sulfate impurities in heparin by capillary electrophoresis.

Recently, oversulfated chondroitin sulfate (OSCS) present in certain lots of heparin was identified as the toxic contaminant responsible for severe side effects following intravenous heparin administration. The United States Pharmacopeia (USP) and European Pharmacopeia (Eur.Ph.