Design and Synthesis of Substrate and Internal Standard Conjugates for Profiling Enzyme Activity in the Sanfilippo Syndrome by Affinity Chromatography/Electrospray Ionization Mass Spectrometry

2001 ◽  
Vol 12 (4) ◽  
pp. 603-615 ◽  
Author(s):  
Scott A. Gerber ◽  
František Tureček ◽  
Michael H. Gelb
2018 ◽  
Vol 16 (1) ◽  
pp. 87-94 ◽  
Author(s):  
O Fayos ◽  
GF Barbero ◽  
M Savirón ◽  
J Orduna ◽  
AG Durán ◽  
...  

AbstractCapsinoids exhibit health-promoting properties and are therefore compounds of interest for medical and food sciences. They are minor compounds present in relatively high concentrations in only a few number of pepper cultivars. It is desirable to quantify capsinoids to provide selected cultivars with high capsinoid contents, which can then be employed as health food product. Quantifying low concentrations of capsinoids from pepper fruit requires a precise and selective analytical technique such as HPLC coupled to electrospray ionization - mass spectrometry, with development of an internal standard essential. In this work, the synthesis method of a novel compound analogue of capsinoids, the (±)-3,4-dimethoxybenzyl-4-methyloctanoate, which could be a suitable internal standard for capsinoid determination by electrospray ionization - mass spectrometry is described.(±)-3,4-dimethoxybenzyl-4-methyloctanoate was stable under the analysis conditions and exerted chemical and physical properties similar to those of capsinoids. This internal standard will provide an accurate capsinoid determination by electrospray ionization - mass spectrometry, thus facilitating the pepper breeding programs, screening pepper cultivars and a better understanding of capsinoid biosynthetic pathway.


Author(s):  
Freneil B. Jariwala ◽  
John A. Hibbs ◽  
Iryna Zhuk ◽  
Svetlana A. Sukhishvili ◽  
Athula B. Attygalle

AbstractAminoglycosides are broad-spectrum antibiotics often employed to combat Gram-negative bacterial infections. A technique based on electrospray-ionization mass spectrometry (ESI-MS) was developed for rapid determination of aminoglycosides. This method, which does not require prior chromatographic separation, or derivatization and extensive sample preparation steps, was deployed to estimate gentamicin, tobramycin, and amikacin in pharmaceutical formulations. Upon gas-phase collisional activation, protonated gentamicin, tobramycin, and amikacin undergo a facile loss of their respective “C” ring moiety to produce characteristic ions of m/z 322, 324, and 425, respectively. The mass spectral peak intensities for these specific product ions were monitored either by a flow-injection analysis selected-ion monitoring (FIA-SIM) time-intensity method or by a mass spectrometric internal-standard method. The linear dynamic ranges of detection for both methods were evaluated to be 10–1000 ng/mL for gentamicin, 25–2500 ng/mL for tobramycin, and 10–1000 ng/mL for amikacin. The internal-standard mass spectrometric method afforded lower intra-day and inter-day variations (2.3–3.0% RSD) compared to those from FIA-SIM method (4.5–5.0% RSD). This method was applied as a potential alternative procedure to determine gentamicin in commercial pharmaceutical samples and to monitor the release of gentamicin from “self-defensive” tannic acid-based layer-by-layer films into phosphate buffer solutions at different pHs.


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