Recent advances in liquid microextraction techniques coupled with MS for determination of small-molecule drugs in biological samples

Bioanalysis ◽  
2012 ◽  
Vol 4 (6) ◽  
pp. 725-739 ◽  
Author(s):  
Mohammad Saraji ◽  
Nasrin Khaje
Keyword(s):  
Small Molecule ◽  
Biological Samples ◽  
Small Molecule Drugs ◽  
Recent Advances ◽  
Microextraction Techniques ◽  
Liquid Microextraction

Dispersive Liquid-Liquid Microextraction Based on Ionic Liquid and Spectrophotometric Determination of Bilirubin in Biological Samples

2020 ◽  
Vol 16 (5) ◽  
pp. 652-659
Author(s):  
Asiye A. Avan ◽  
Hayati Filik
Keyword(s):  
Ionic Liquid ◽  
Ionic Liquids ◽  
Biological Samples ◽  
Urine Samples ◽  
Spectrophotometric Detection ◽  
Full Color ◽  
Dispersive Liquid Liquid Microextraction ◽  
Urine And Serum ◽  
Liquid Microextraction

Background: An Ionic Liquid-based based Dispersive Liquid-Liquid Microextraction (IL-DLLME) method was not applied to preconcentration and determination of bilirubin. Ionic Liquids (ILs) are new chemical compounds. In recent years, Ionic Liquids (ILs) have been employed as alternative solvents to toxic organic solvents. Due to these perfect properties, ILs have already been applied in many analytical extraction processes, presenting high extraction yield and selectivity for analytes. Methods: In this study, IL-DLLME was applied to biological samples (urine and serum) for the spectrophotometric detection of bilirubin. For bilirubin analysis, the full-color development was based on the reaction with periodate in the presence of hydrochloric acid. The high affinity of bilirubin for the ionic liquid phase gave extraction percentages above 98% in 0.3 M HCl solution. Results: Several IL-extraction parameters were optimized and room temperature ionic liquid 1-butyl- 1-methylpyrrolidinium bis(trifluoromethylsulfonyl)imide and ethanol were used as extraction and disperser solution. The linear range was found in the range of 0.5-6.0 μM (0.3-3.5 μg mL-1) and the limits of detection of the proposed method was 0.5 μM (0.3 μg mL-1). The proposed method was applied for the preconcentration and separation of trace bilirubin in real urine samples. Also, the recoveries for bilirubin in spiked biological samples (urine and serum) were found to be acceptable, between 95-102%. Conclusion: The proposed IL-DLLMEapproach was employed for the enrichment and determination of trace levels of bilirubin in urine samples using NaIO4 as an oxidizing agent and Uv-vis spectrophotometric detection. The periodate oxidation of bilirubin is rapid, effective, selective, and simple to perform. The method contains only HCl, NaOI4, and an anionic surfactant. The method may be useful for economizing in the consumption of reagents in bilirubin determining. The IL-DLLMEmethod ensures a high yield and has a low toxicity no skin sensitization, no mutagenicity and no ecotoxicity in an aquatic environment since only very low quantities of an IL is required. For full-color formation, no any extra auxiliary reagents are required. Besides, the IL-DLLME technique uses a low-cost instrument such as Uv-vis which is present in most of the medical laboratories.

scholarly journals Bioanalysis of small-molecule drugs in nasal and paranasal tissues and secretions: Current status and perspectives

2012 ◽  
Vol 10 (3) ◽  
pp. 686-702
Author(s):  
Ana Serralheiro ◽  
Gilberto Alves ◽  
Amílcar Falcão
Keyword(s):  
Central Nervous System ◽  
Nervous System ◽  
Small Molecule ◽  
Intranasal Administration ◽  
Quantitative Measurement ◽  
Current Status ◽  
Small Molecule Drugs ◽  
Development And Validation ◽  
Liquid Chromatographic

AbstractOver the last years, interest in intranasal administration as an alternative and promising route for the delivery of drugs withlocal, systemic, and even central nervous system action has tremendously increased. Accordingly, understanding of the propertiesand characteristics of the nasal cavity as well as the biodisposition processes of drugs into the nasal compartments is acquiringa significant prominence in the field of pharmacology. In this context, the development and validation of bioanalytical methodologies for the quantitative measurement of drugs and their metabolites in nasal and paranasal tissues and/or secretions is of the utmostimportance. However, currently, information concerning bioanalysis of drugs in nasal and paranasal tissues and/or secretionsis scattered. This review aims to provide a valuable overview of the methodologies that have been used for the collectionand preparation of nasal and paranasal samples with special emphasis placed on the review of liquid chromatographic methodsemployed for the quantitative determination of small-molecule drugs and their metabolites in such specimens.

scholarly journals Sensitive Determination of Terazosin in Pharmaceutical Formulations and Biological Samples by Ionic-Liquid Microextraction Prior to Spectrofluorimetry

2012 ◽  
Vol 2012 ◽  
pp. 1-7 ◽  
Author(s):  
Mohsen Zeeb ◽  
Mahdi Sadeghi
Keyword(s):  
Ionic Liquid ◽  
Ionic Strength ◽  
Biological Samples ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Experimental Conditions ◽  
Relative Standard ◽  
Common Ion ◽  
Liquid Microextraction

An efficient and environmentally friendly sample preparation method based on the application of hydrophobic 1-Hexylpyridinium hexafluorophosphate [Hpy][PF6] ionic liquid (IL) as a microextraction solvent was proposed to preconcentrate terazosin. The performance of the microextraction method was improved by introducing a common ion of pyridinium IL into the sample solution. Due to the presence of the common ion, the solubility of IL significantly decreased. As a result, the phase separation successfully occurred even at high ionic strength, and the volume of the settled IL-phase was not influenced by variations in the ionic strength (up to 30% w/v). After preconcentration step, the enriched phase was introduced to the spectrofluorimeter for the determination of terazosin. The obtained results revealed that this system did not suffer from the limitations of that in conventional ionic-liquid microextraction. Under optimum experimental conditions, the proposed method provided a limit of detection (LOD) of 0.027 μg L−1and a relative standard deviation (R.S.D.) of 2.4%. The present method was successfully applied to terazosin determination in actual pharmaceutical formulations and biological samples. Considering the large variety of ionic liquids, the proposed microextraction method earns many merits, and will present a wide application in the future.

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