A General, Positive Ion Mode ESI-MS Approach for the Analysis of Singly Charged Inorganic and Organic Anions Using a Dicationic Reagent

2007 ◽  
Vol 79 (19) ◽  
pp. 7346-7352 ◽  
Author(s):  
Renee J. Soukup-Hein ◽  
Jeffrey W. Remsburg ◽  
Purnendu K. Dasgupta ◽  
Daniel W. Armstrong
2009 ◽  
Vol 30 (22) ◽  
pp. 3918-3925 ◽  
Author(s):  
Xiuli Lin ◽  
Anthony R. Gerardi ◽  
Zachary S. Breitbach ◽  
Daniel W. Armstrong ◽  
Christa L. Colyer

2014 ◽  
Vol 97 (6) ◽  
pp. 1497-1502 ◽  
Author(s):  
Dada Patil ◽  
Manish Gautam ◽  
Sunil Gairola ◽  
Suresh Jadhav ◽  
Bhushan Patwardhan

Abstract Asparagus racemosus (AR) is a popular botanical present in several Ayurvedic medicines and nutritional and dietary supplements with immunomodulatory, galactogogue, and anticancer activity. A steroidal saponin known as shatavarin IV is one of the active constituents of AR. A new, selective, and rapid HPLC/MS/MS method has been developed and validated for quantitative estimation of shatavarin IV in crude, processed, and marketed samples of AR. The analytes were separated on a Luna C18 column using simple isocratic elution with water (0.1% acetic acid)–acetonitrile (0.1% acetic acid; 70 + 30, v/v) at a flow rate of 0.8 mL/min. The analytes were detected by electrospray ionization (ESI)-MS/MS and quantified using multiple reaction monitoring techniques in the positive ion mode. The method showed excellent linearity (r2 > 0.998) over the concentration range of 7.5 to 254 ng/mL with LOD of 2.5 ng/mL. Precision (RSD) and accuracy (recovery) were found in the ranges of 2.00 to 5.15 and 102 to 110%, respectively. The validated HPLC/ESI-MS/MS method was successfully applied to the quantification of shatavarin IV in crude, processed, and marketed (single or multiherb) AR samples. Therefore, this method could be used for QC and standardization of pharmaceutical or nutritional products containing AR.


2011 ◽  
Vol 879 (17-18) ◽  
pp. 1393-1401 ◽  
Author(s):  
A. Kretschmer ◽  
M. Giera ◽  
M. Wijtmans ◽  
L. de Vries ◽  
H. Lingeman ◽  
...  
Keyword(s):  
Esi Ms ◽  

2015 ◽  
Vol 13 (1) ◽  
Author(s):  
Roxana M. Ghiulai ◽  
Mirela Sarbu ◽  
Constantin Ilie ◽  
Alina D. Zamfir

AbstractStructural analysis of long chain polysaccharides by electrospray ionization mass spectrometry (ESI-MS) is challenging since these molecules do not contain readily ionizable groups. Their mass spectra are dominated by singly charged ions, limiting the detection of high molecular weight species. Derivatization can enhance ionization, but analyte loss on purification decreases sensitivity. We report a method based on nanoESI-MS and MS/MS by collision induced dissociation (CID) for underivatized long chain polysaccharides. The procedure was tested on underivatized polydisperse dextrans (average molecular weight 4,000) at 2.6 kV ESI voltage and CID MS/MS at energies between 30-60 eV. 113 ions corresponding to species from Glc2 to Glc35 were detected. Ions at m/z 1,409.48, 1,107.35 and 1,438.47, assigned to [G17+2Na]2+,[G20+H+Na+K]3+ and [G35+2H+Na+K]4+, were sequenced and characterized by MS/MS. The component containing 35 Glc repeats is the longest polysaccharide chain detected by ESI-MS and structurally analyzed by MS/MS without prior derivatization and/or separation.


1998 ◽  
Vol 76 (2) ◽  
pp. 194-198
Author(s):  
Costas Stathakis ◽  
Richard M Cassidy

The capillary electrophoretic separation of iodide, nitrate, perchlorate, thiocyanate, bromate, iodate, and ethane-, butane-, pentane-, and octanesulphonate was examined in sodium chromate or potassium hydrogen phthalate electrolytes and in the presence of α -, γ -, (0-40 mmol/L) and β -cyclodextrin (0-10 mmol/L). Largest decreases in electrophoretic mobility were observed for iodide, perchlorate, and thiocyanate, probably due to inclusion of these anions in the cyclodextrin (CD) cavity. Changes in migration patterns and electroosmotic flow were observed, which depended on cyclodextrin type and concentration and on electrolyte-cyclodextrin interactions. Thus for larger cavity cyclodextrins ( β-or γ-cyclodextrin) or in the presence of chromate, relatively small decreases in electrophoretic mobilities for all the anions were observed, indicating that a good match between analyte and cavity size and minimal cyclodextrin affinity for electrolyte ions are essential for different migration patterns. Separation efficiencies were between 50 000 and 400 000 theoretical plates, and calibration plots for iodide and octanesulphonate were linear; R2 = 0.998 and 0.9999, respectively, in the concentration range (5 x 10-5)-(5 x 10-3) mol/L.Key words: capillary electrophoresis, inorganic and organic anions, cyclodextrins, inclusion complex, electroosmotic flow control.


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