Quantitative Capillary Electrophoresis/Ion Spray Tandem Mass Spectrometry Determination of EDTA in Human Plasma and Urine

Abstract

A quantitative method has been developed for the determination of EDTA in human plasma and urine. The samples are prepared with automated anion-exchange solid-phase extraction using 100 microL of human plasma. The extracts are analyzed by capillary electrophoresis/mass spectrometry using selected reaction monitoring in the negative ion mode. Large-volume injections (10% of the CE capillary volume) are used to improve the concentration level of detection via field-amplified sample injection. The first reported validation of a CE/MS/MS technique was carried out for this method. Using a 13C stable-label isotope for the internal standard, the lower level of detection and lower level of quantitation were determined to be 7.3 and 14.6 ng/mL EDTA in human plasma, respectively. The injection precision had a relative standard deviation (RSD) of 6.1%. The intra-assay precision was less than 15% RSD. The intra-assay accuracy was less than +/- 12% bias from the nominal concentration. The interassay precision was less than 18% RSD and the interassay accuracy was less than +/- 9% bias from the nominal concentration.

Homemade Capillary Electrophoresis Coupled to a Mass Spectrometer

“…However, this setup has some disadvantages, such as i) the electrode tends to form bubbles due to electrochemical reactions (electrolysis) on its surface, causing problems such as the interruption of the electric field in the CE system; ii) the occurrence of redox reactions due to the relatively large area of the capillary; and iii) the dead volume at the junction between the capillaries causes increased dispersion due to flow disturbance. [22,23] …”

Eletroforese capilar acoplada à espectrometria de massas (CE-MS): vinte anos de desenvolvimento

“…A análise do entorpecente ecstasy e seus derivados em urina, usando CE-ESI-MS, também é encontrada na literatura. 100 Demais fármacos como cafeína, anfetamina e benzodiazepinas também já foram analisados pela técnica de CE-MS. [101][102][103][104] Metodologias via CE-MS para analisar proteínas glico-conjugadas em urina de pacientes foram também desenvolvidas, as quais auxiliam o diagnóstico de várias desordens metabólicas, tais como Diabete mellitus e outras doenças que afetam o metabolismo em geral.…”

18 Coupling CE and microchip-based devices with mass spectrometry

“…126,173,2912293 This subject is however of prime importance, particularly for the pharmaceutical industry where the reliability of analytical data is essential. For this reason, method development is generally followed by an evaluation of quantitative performance using an appropriate validation procedure performed in agreement with criteria established by the International Conference on Harmonisation of technical requirements for registration of pharmaceuticals for human use (ICH) and the Food and Drug Administraction (FDA) guidelines, or Société Franc -aise des Sciences et Techniques Pharmaceutiques (SFSTP) commissions.…”