Accession Number : ADA290265

Title :   Analysis of Saxitoxin from Urine Using Continuous Flow Fast Atom Bombardment and Electrospray Ionization Mass Spectrometry.

Descriptive Note : Final rept. 1 Apr 92-30 Jun 94,

Corporate Author : MINNESOTA UNIV MINNEAPOLIS

Personal Author(s) : Mirocha, Chester J.

PDF Url : ADA290265

Report Date : 30 JUL 1994

Pagination or Media Count : 66

Abstract : A method of analysis for saxitoxin (STX) in the rat (blood serum and urine) and human urine was developed using CBA and EMPORE columns followed by oxidation with hydrogen peroxide and analysis by HPLC using a C18 reversed phase column and detection by fluorescence of the OPA derivative. Detection was also made by continuous flow fast atom bombardment (CF/FAB/MS). STX was found in the serum and urine of rats treated with STX (1 to 3 microns g total intraperitoneal injection) as soon as 10 min after dosing and up to 8 hrs. Rats dosed with 75 microns g by stomach intubation had detectable amounts of STX in their urine for up to 31 hrs. Confirmation was done by CF/FAB/MS using selected ion monitoring (m/z+ 300 & 282). The limit of detection by HPLC was 4 ppb in human urine and 220 ppb in rat urine. The limit of detection by CF/FAB/MS was 25 ppb in human urine. A method of analysis using EMPORE column technology yielded a percent recovery of 102 at 25 ppb and 99 at 50 ppb. CBA columns used for comparison gave a percent recovery that varied between 64 and 90%.

Descriptors :   *IONIZATION, *URINE, *MASS SPECTROMETRY, IONS, DETECTION, FLUORESCENCE, RATS, MONITORING, HUMANS, METABOLISM, OXIDATION, INTRAMUSCULAR INJECTIONS, PERITONEUM, BLOOD SERUM, SPRAYS, HYDROGEN PEROXIDE, INTUBATION, STOMACH.

Subject Categories : Nuclear Physics & Elementary Particle Physics
      Inorganic Chemistry

Distribution Statement : APPROVED FOR PUBLIC RELEASE