Current developments in LC-MS for pharmaceutical analysis

Beccaria, Marco; Cabooter, Deirdre

doi:10.1039/c9an02145k

Cited by 155 publications

(96 citation statements)

References 154 publications

(150 reference statements)

Supporting

Mentioning

Contrasting

Unclassified

Order By: Relevance

“…The structures of these ions are shown on Supplementary Figs. 4(a) and 3(a) correspondingly. Under atmospheric conditions, in the mass spectrum they manifest themselves as fragmentary ions М⋅[M-R] + with m/z 335 and as cluster ones М⋅[M-H] + with m/z 553.…”

Section: Resultsmentioning

confidence: 99%

“…2 Different methods of ionization from traditional electron ionization coupled with gas chromatography (GC) to high performance liquid chromatography (HPLC) coupled with tandem mass spectrometry, electrospray ionization and chemical ionization under air atmosphere. [3][4][5][6][7] Hayen and Karst investigated electrochemical transformation of phenothiazine and its derivatives after liquid chromatographic separation using mass spectrometry and fluorescence spectroscopy. 8 In an electrochemical cell consisting of porous carbon glass, phenothiazines are easily transformed into oxidized products detectable by online fluorescence spectroscopy and mass spectrometry.…”

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

Examination of the effect of air atmosphere on heterogeneous reactions under surface ionization of psychotropic drug molecules

Khasanov

Iskhakova

Usmanov

2020

Eur J Mass Spectrom (Chichester)

View full text Add to dashboard Cite

The results of mass spectrometric studies of surface ionization of molecules of psychotropic drugs such as chlorpromazine, amitriptyline and medazepam in an air atmosphere have been presented. The channels of heterogeneous reactions occurring during the molecule adsorption on the hot surface of the thermoemitter from refractory metal oxides have been revealed, as well as the influence of air atmosphere on these reactions. A strong influence of the air atmosphere on the heterogeneous association reactions with the emission of [M + H]+ ions has been found. This ion line is the main in the mass spectra of all the substances under study instead of the characteristic main line in the surface ionization mass spectra obtained in vacuum. The effect of air on the reactions of dehydrogenation and dissociation of adsorbed molecules of organic compounds has been insignificant. In the surface ionization mass spectra of all the substances studied under atmospheric conditions the adduct cluster ions М⋅[М−R]+, М⋅[М−Н]+ and М⋅[М+Н]+ (where М is the molecule, R is the radical, H is the hydrogen atom) up to М⋅[М+Н]+⋅HCl. They are probably formed by adhesion of analyte molecules to the primary ions [М−R]+, [М−Н]+ and [М+Н]+. A comparative analysis has been also performed with the data obtained by chromato-mass spectrometry with electron ionization, as well as with the surface ionization data for these preparations obtained under high vacuum.

show abstract

Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

Examination of the effect of air atmosphere on heterogeneous reactions under surface ionization of psychotropic drug molecules

Khasanov

Iskhakova

Usmanov

2020

Eur J Mass Spectrom (Chichester)

View full text Add to dashboard Cite

show abstract

“…In this area, LC or GC coupled to HRMS has been widely applied in the identification of transformation products, with time-of-flight (TOF), quadrupole-TOF (QTOF), and Orbitrap mass spectrometers increasing in use. These techniques were used in the study of the behavior of PhACs, the identification of their transformation or degradation products in wastewaters, natural waters, and drinking waters [51,55,56].…”

Section: Introductionmentioning

confidence: 99%

Overview of Sample Preparation and Chromatographic Methods to Analysis Pharmaceutical Active Compounds in Waters Matrices

Almeida

2021

Separations

View full text Add to dashboard Cite

In the environment, pharmaceutical residues are a field of particular interest due to the adverse effects to either human health or aquatic and soil environment. Because of the diversity of these compounds, at least 3000 substances were identified and categorized into 49 different therapeutic classes, and several actions are urgently required at multiple steps, the main ones: (i) occurrence studies of pharmaceutical active compounds (PhACs) in the water cycle; (ii) the analysis of the potential impact of their introduction into the aquatic environment; (iii) the removal/degradation of the pharmaceutical compounds; and, (iv) the development of more sensible and selective analytical methods to their monitorization. This review aims to present the current state-of-the-art sample preparation methods and chromatographic analysis applied to the study of PhACs in water matrices by pinpointing their advantages and drawbacks. Because it is almost impossible to be comprehensive in all PhACs, instruments, extraction techniques, and applications, this overview focuses on works that were published in the last ten years, mainly those applicable to water matrices.

show abstract

“…Liquid chromatography-mass spectrometry (LC-MS) is a rapidly developing technology that is widely used for pharmaceuticals development and evaluation. 4 On the other hand, a comprehensive review concludes that there is no impeccable method yet to be found. Among analytical instrumental techniques used in the analysis of degradation products and impurity profiling during the period 2013-2017, LC-MS appears to be the most common technique.…”

Section: Introductionmentioning

confidence: 99%

Analysis of impurities in pharmaceuticals by LC‐MS with cold electron ionization

2020

View full text Add to dashboard Cite

Pharmaceuticals require careful and precise determination of their impurities that might harm the user upon consumption. Although today, the most common technique for impurities identification is liquid chromatography-mass spectrometry (LC-MS/MS), it has several downsides due to the nature of the ionization method. Also, the analyses in many cases are targeted thus despite being present, some of the compounds will not be revealed. In this paper, we propose and show a new method for untargeted analysis and identification of impurities in active pharmaceutical ingredients (APIs). The instrument used for these analyses is a novel electron ionization (EI) LC-MS with supersonic molecular beams (SMB). The EI-LC-MS-SMB was implemented for analyses of several drug samples spiked with an impurity. The instrument provides EI mass spectra with enhanced molecular ions, named Cold EI, which increases the identification probabilities when the compound is identified with the aid of an EI library like National Institute of Standards and Technology (NIST). We analyzed ibuprofen and its impurities, and both the API and the expected impurity were identified with names and structures by the NIST library. Moreover, other unexpected impurities were found and identified proving the ability of the EI-LC-MS-SMB system for truly untargeted analysis. The results show a broad dynamic range of four orders of magnitude at the same run with a signal-to-noise ratio of over 10 000 for the API and almost uniform response.

show abstract

Current developments in LC-MS for pharmaceutical analysis

Abstract: Liquid chromatography (LC) based techniques in combination with mass spectrometry (MS) detection have had a large impact on the development of new pharmaceuticals in the past decades.

Cited by 155 publications

References 154 publications

Examination of the effect of air atmosphere on heterogeneous reactions under surface ionization of psychotropic drug molecules

Examination of the effect of air atmosphere on heterogeneous reactions under surface ionization of psychotropic drug molecules

Overview of Sample Preparation and Chromatographic Methods to Analysis Pharmaceutical Active Compounds in Waters Matrices

Analysis of impurities in pharmaceuticals by LC‐MS with cold electron ionization

Contact Info

Product

Resources

About