title: Determination of sulpiride by capillary electrophoresis with end-column electrogenerated chemiluminescence detection.
abstract: BACKGROUND
  Capillary electrophoresis (CE) with tris(2,2'-bipyridyl)ruthenium(II) [Ru(bpy)3(2+)]-electrogenerated chemiluminescence (ECL) detection is a promising method for clinical analysis. In this study, a method combining CE with Ru(bpy)3(2+) ECL (CE-ECL) detection that can be applied to amine-containing clinical species was developed, and the performance of CE-ECL as a quantitative method for determination of sulpiride in human plasma or urine was evaluated.
  
  
  METHODS
  Sulpiride was separated by capillary zone electrophoresis in uncoated fused-silica capillaries [50 cm x 25 microm (i.d.)] filled with phosphate buffer (pH 8.0) and a driving voltage of +15 kV, with end-column Ru(bpy)3(2+) ECL detection. A platinum disc electrode was used as working electrode. Sulpiride in human plasma or urine samples (100 microL) was extracted by a double-step liquid-liquid extraction procedure, dried under nitrogen at 35 degrees C in a water bath, and reconstituted with 100 microL of filtered water. The extraction solvent was ethyl acetate-dichloromethane (5:1 by volume).
  
  
  RESULTS
  Under optimum conditions (pH 8.0 phosphate buffer, injection for 6 s at 10 kV, and +1.2 V as detection potential), separation of sulpiride was accomplished within 4 min. The calibration curve was linear over a concentration range of 0.05-25.0 micromol/L, and the limit of detection was 2.9 x 10(-8) mol/L for sulpiride. Intra- and interday CVs for ECL intensities were <6%. Extraction recoveries of sulpiride were 95.6-101% with CVs of 2.9-6.0%. The method was clinically validated for patient plasma and urine samples.
  
  
  CONCLUSIONS
  CE combined with Ru(bpy)3(2+) ECL is reproducible, precise, selective, and enables the analysis of sulpiride in human plasma and urine. It thus is of value for rapid and efficient analysis of amine-containing analytes of clinical interest.
authors.affiliation: State Key Laboratory of Electroanalytical Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun, Jilin 130022, People's Republic of China.
authors.forename: Jifeng
authors.initials: J
authors.lastname: Liu
authors.forename: Weidong
authors.initials: W
authors.lastname: Cao
authors.forename: Haibo
authors.initials: H
authors.lastname: Qiu
authors.forename: Xiuhua
authors.initials: X
authors.lastname: Sun
authors.forename: Xiurong
authors.initials: X
authors.lastname: Yang
authors.forename: Erkang
authors.initials: E
authors.lastname: Wang
mesh_terms: D015082:2,2'-Dipyridyl / Q000031:analogs & derivatives* / Q000737:chemistry; D000085:Acetates; D000328:Adult; D018687:Antidepressive Agents, Second-Generation / Q000032:analysis* / Q000097:blood / Q000652:urine; D014150:Antipsychotic Agents / Q000032:analysis* / Q000097:blood / Q000652:urine; D018492:Dopamine Antagonists / Q000032:analysis* / Q000097:blood / Q000652:urine; D004563:Electrochemistry; D019075:Electrophoresis, Capillary; D006801:Humans; D008163:Luminescent Measurements; D008752:Methylene Chloride; D008875:Middle Aged; D009942:Organometallic Compounds / Q000737:chemistry; D017448:Receptors, Dopamine D2 / Q000187:drug effects; D012428:Ruthenium; D012997:Solvents; D013469:Sulpiride / Q000032:analysis* / Q000097:blood / Q000652:urine
chemical_list: D000085:Acetates; D018687:Antidepressive Agents, Second-Generation; D014150:Antipsychotic Agents; D018492:Dopamine Antagonists; D009942:Organometallic Compounds; D017448:Receptors, Dopamine D2; D012997:Solvents; C058901:tris(2,2'-bipyridine)ruthenium III; D015082:2,2'-Dipyridyl; D008752:Methylene Chloride; C007650:ethyl acetate; D013469:Sulpiride; D012428:Ruthenium