scholarly journals APPLICATION OF LIQUID CHROMATOGRAPHY COUPLED WITH MASS SPECTROMETRY IN THE IMPURITY PROFILING OF DRUG SUBSTANCES AND PRODUCTS

Author(s):  
Akshatha H S ◽  
Gurupadayya Bm

As the drug safety and efficacy is hampered in the presence of an impurity, the international regulatory agencies laid down stringent limits for the control of impurities in the active pharmaceutical ingredient and pharmaceutical formulations. The conventional approaches lack the characterization of impurities in trace levels, due to sensitivity issues, hyphenated techniques are preferred. Among the modern hyphenated techniques, liquid chromatography-mass spectrometry (LC-MS) has high sensitivity and can analyze large number of organic compounds in a short period of time. In the present study, the impurity profiling of various drug substances and products using LC-MS about past 6 years were retrospect for its importance, instrumentations, and applications.

Separations ◽  
2021 ◽  
Vol 8 (2) ◽  
pp. 18
Author(s):  
Emanuela Trovato ◽  
Adriana Arigò ◽  
Federica Vento ◽  
Giuseppe Micalizzi ◽  
Paola Dugo ◽  
...  

In the last few years, the flavored beer market has increased significantly. In particular, consumers showed a growing interest in citrus-flavored beers. Citrus fruits contain, among other class of compounds, terpenes and terpenoids and oxygenated heterocyclic compounds. The absence of a specific legislation concerning beer flavored production and ingredients reported on the labels makes these beers subject to possible adulterations. Solid phase micro extraction (SPME) followed by gas chromatographic–mass spectrometry (GC-MS) and gas chromatographic-flame ionization detector (GC-FID) analysis of the volatile profile together with the characterization of the oxygen heterocyclic compounds through high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS) demonstrated to be a powerful analytical strategy for quality control. In this study, we combined the volatile and non-volatile profiles of “citrus flavored mainstream beers”, in order to evaluate the authenticity and determine markers to prevent food frauds. The changes in the aroma composition of the unflavored types after the addition of peel, or citrus essential oil were also evaluated. The linear retention index (LRI) system was used for both techniques; in particular, its application in liquid chromatography is still limited and represents a novelty. The coupling of the high sensitivity of the HPLC MS/MS method with the LRI system, it has made possible for the first time a reliable identification and an accurate quantification of furocoumarins in citrus-flavored beers.


2020 ◽  
Vol 17 (1) ◽  
pp. 31-39
Author(s):  
Marilene Lopes Ângelo ◽  
Fernanda de Lima Moreira ◽  
Ana Laura Araújo Santos ◽  
Hérida Regina Nunes Salgado ◽  
Magali Benjamim de Araújo

Background:: Tibolone is a synthetic steroid commercialized by Organon under the brand name Livial (Org OD14), which is used in hormone therapy for menopause management and treatment of postmenopausal osteoporosis. Tibolone is defined as a selective tissue estrogenic activity regulator (STEAR) demonstrating tissue-specific effects on several organs such as brain, breast, urogenital tract, endometrium, bone and cardiovascular system. Aims:: This work aims to (1) present an overview of important published literature on existing methods for the analysis of tibolone and/or its metabolites in pharmaceutical formulations and biological fluids and (2) to conduct a critical comparison of the analytical methods used in doping control, pharmacokinetics and pharmaceutical formulations analysis of tibolone and its metabolites. Results and conclusions: : The major analytical method described for the analysis of tibolone in pharmaceutical formulations is High Pressure Liquid Chromatography (HPLC) coupled with ultraviolet (UV) detection, while Liquid Chromatography (LC) or Gas Chromatography (GC) used in combination with Mass Spectrometry (MS) or tandem mass spectrometry (MS/MS) is employed for the analysis of tibolone and/or its metabolites in biological fluids.


Separations ◽  
2021 ◽  
Vol 8 (3) ◽  
pp. 33
Author(s):  
Xavier Garcia ◽  
Maria del Mar Sabaté ◽  
Jorge Aubets ◽  
Josep Maria Jansat ◽  
Sonia Sentellas

This paper aims to cover the main strategies based on ion mobility spectrometry (IMS) for the analysis of biological samples. The determination of endogenous and exogenous compounds in such samples is important for the understanding of the health status of individuals. For this reason, the development of new approaches that can be complementary to the ones already established (mainly based on liquid chromatography coupled to mass spectrometry) is welcomed. In this regard, ion mobility spectrometry has appeared in the analytical scenario as a powerful technique for the separation and characterization of compounds based on their mobility. IMS has been used in several areas taking advantage of its orthogonality with other analytical separation techniques, such as liquid chromatography, gas chromatography, capillary electrophoresis, or supercritical fluid chromatography. Bioanalysis is not one of the areas where IMS has been more extensively applied. However, over the last years, the interest in using this approach for the analysis of biological samples has clearly increased. This paper introduces the reader to the principles controlling the separation in IMS and reviews recent applications using this technique in the field of bioanalysis.


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