Purification of pharmaceutical preparations using thin-layer chromatography to obtain mass spectra with Direct Analysis in Real Time and accurate mass spectrometry

2011 ◽  
Vol 3 (6) ◽  
pp. 345-351 ◽  
Author(s):  
Jessica L. Wood ◽  
Robert R. Steiner
Keyword(s):  
Mass Spectrometry ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Real Time ◽  
Mass Spectra ◽  
Pharmaceutical Preparations ◽  
Direct Analysis ◽  
Accurate Mass ◽  
Accurate Mass Spectrometry ◽  
Layer Chromatography

scholarly journals Assessment of direct analysis in real time accurate mass spectrometry for the determination of triclosan in complex matrices

2021 ◽  
Author(s):  
M. Cobo-Golpe ◽  
J. García-Martín ◽  
M. Ramil ◽  
R. Cela ◽  
I. Rodríguez
Keyword(s):  
Mass Spectrometry ◽  
Real Time ◽  
Personal Care Products ◽  
Direct Analysis ◽  
Accurate Mass ◽  
Personal Care ◽  
Complex Matrices ◽  
Accurate Mass Spectrometry ◽  
Tof Ms

AbstractIn this work, the applicability of direct analysis in real time coupled to accurate mass spectrometry (DART-MS) to the quantitative determination of triclosan (TCS) in samples with increasing complexity, from personal care products to extracts from sewage, is investigated. In the first term, DART-MS spectra of TCS as free phenol and as derivatized species are characterized; thereafter, the effects of several instrumental variables in the detectability of TCS (i.e., temperature, solvent, and compound holder) are discussed. Under final selected conditions, TCS was determined from its [M-H]− ions, without need of derivatization, attaining an instrumental limit of quantification of 5 ng mL−1, with a linear response range up to 1000 ng mL−1. Complex matrices, such as solid-phase extracts obtained from environmental water samples, moderately inhibited the ionization efficiency of TCS, with signal attenuation percentages in the range of 6 to 57%, depending on the sample type and on the concentration factor provided by the SPE procedure. The accuracy of results obtained by DART-MS was evaluated using liquid chromatography (LC) with MS detection; in both cases, a time-of-flight (TOF) MS instrument was employed for the selective determination of the [M−H]− ions of TCS (m/z values 286.9439 and 288.9410) using a mass window of 20 ppm. DART-MS did not only provide enough sensitivity to detect the presence of TCS in environmental samples (raw and treated wastewater as well as freeze-dried sludge), but also measured concentrations matched those determined by LC-ESI-TOF-MS, with only slightly higher standard deviations. During analysis of personal care products, containing much higher concentrations of TCS in a less complex matrix, both techniques were equivalent in terms of accuracy and precision.

Direct analysis of thin-layer chromatography spots by fast atom bombardment mass spectrometry

1984 ◽  
Vol 56 (1) ◽  
pp. 109-111 ◽  
Author(s):  
Ted. T. Chang ◽  
Jackson O. Lay ◽  
Rudolph J. Francel
Keyword(s):  
Mass Spectrometry ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Fast Atom Bombardment ◽  
Direct Analysis ◽  
Layer Chromatography
Sign in / Sign up

Export Citation Format

Share Document