We describe a method for quantifying diacylglycerols as their 1-pentafluorobenzoyl-2-acyl-3-acetyl-glycerol derivatives by capillary gas chromatography-negative ion chemical ionization-mass spectrometry. The basis of the method resides in the sequential treatment of diacylglycerols with acetic anhyd
Quantification of Jasmonic Acid by Capillary Gas Chromatography-Negative Chemical Ionization-Mass Spectrometry
โ Scribed by M.J. Mueller; W. Brodschelm
- Publisher
- Elsevier Science
- Year
- 1994
- Tongue
- English
- Weight
- 949 KB
- Volume
- 218
- Category
- Article
- ISSN
- 0003-2697
No coin nor oath required. For personal study only.
โฆ Synopsis
Jasmonic acid can be assayed by the highly sensitive and reproducible gas chromatography-negative ion chemical ionization-mass spectrometry (GC-NICI-MS) technique. We describe an optimized sample preparation method for routine analysis of jasmonic acids which allows the analysis of more than 10 samples/day. The basis of the method resides in a one-step extraction and phase partition, selective adsorption/elution of acids with an aminopropyl column, conversion of acids to pentafluorobenzyl esters, final purification using a silica column, and GC-NICI-MS. Extracted standard curves were linear over an assay range of 1 to 1000 ng; correlation coefficients were typically greater than 0.9999. The limit of detection was 500 fg (2.4 fmol) jasmonic acid/injection at a signal to noise ratio of 10:1. Furthermore, the method was modified for steric analysis of jasmonic acid stereoisomers at the nanogram level. (3R,7S)-(+)-7-Iso-jasmonic acid was found to be biosynthesized from plant tissue cell cultures upon elicitation. This stereoisomer epimerizes rapidly under alkaline and acidic conditions and in the presence of albumin. Epimerization rate constants were determined at different pH values.
๐ SIMILAR VOLUMES
Because of its high sensitivity, gas chromatography negative ion chemical ionization mass spectrometry (GC-NCI-MS) is a potentially valuable analytical tool for the stndy of cholesterol metabolism. Of several derivatives prepared for potential use in tracer studies pentafluorobenzoyl cholesterol was
A negative ion chemical ionization (NICI) gas chromatographic/mass spectrometric method is described for the identification of 15 valproic acid (VPA) metabolites as their pentafluorobenzyl derivatives. Samples analyzed were serum, urine and saliva taken from a volunteer on VPA at steady state and al
Gas chromatography-negative chemical ionization mass spectrometry (GC-NCIMS) has been applied to the analysis of 0-and S-glucuronides. The glucuronides were derivatized with pentafluorobenzyl (PFB) bromide and Tri-Sil, and analyzed by GC-NCIMS. All glucuronides gave a large [M-PFBI-ion indicative of