Microextraction and Chromatographic Analysis of Budesonide Epimers in Exhaled Breath Condensate

2020 ◽  
Vol 16 (8) ◽  
pp. 1032-1040
Author(s):  
Laleh Samini ◽  
Maryam Khoubnasabjafari ◽  
Mohamad M. Alimorad ◽  
Vahid Jouyban-Gharamaleki ◽  
Hak-Kim Chan ◽  
...  

Background: Analysis of drug concentrations in biological fluids is required in clinical sciences for various purposes. Among other biological samples, exhaled breath condensate (EBC) is a potential sample for follow up of drug concentrations. Methods: A dispersive liquid-liquid microextraction (DLLME) procedure followed by a validated liquid chromatography method was employed for the determination of budesonide (BDS) in EBC samples collected using a homemade setup. EBC is a non-invasive biological sample with possible applications for monitoring drug concentrations. The proposed analytical method is validated according to the FDA guidelines using EBC-spiked samples. Its applicability is tested on EBC samples collected from healthy volunteers receiving a single puff of BDS. Results: The best DLLME conditions involved the use of methanol (1 mL) as a disperser solvent, chloroform (200 μL) as an extraction solvent, and centrifugation rate of 3500 rpm for 5 minutes. The method was validated over a concentration range of 21-210 μg·L-1 in EBC. Inter- and intra-day precisions were less than 10% where the acceptable levels are less than 20%. The validated method was successfully applied for the determination of BDS in EBC samples. Conclusion: The findings of this study indicate that the developed method can be used for the extraction and quantification of BDS in EBC samples using a low cost method.

2015 ◽  
Vol 18 (2) ◽  
pp. 207 ◽  
Author(s):  
Maryam Khoubnasabjafari ◽  
Khalil Ansarin ◽  
Vahid Jouyban-Gharamaleki ◽  
Vahid Panahi-Azar ◽  
Ali Shayanfar ◽  
...  

Purpose. A combined microextraction and separation method is presented for the determination of methadone in exhaled breath condensate (EBC) which is a promising non-invasive biological component for monitoring drug concentrations. Methods. In this work, dispersive liquid–liquid microextraction (DLLME) and ultrasonic liquid–liquid microextraction (ULLME) procedure coupled with a validated liquid chromatography method were used for analysis of methadone in EBC collected using an in-house cold trap setup. The method has been validated according to the FDA guidelines using EBC-spiked samples and tested on a number of EBC samples collected from patients. Results. The best DLLME conditions involved the use of a disperser solvent of methanol (1 mL), extraction solvent of chloroform (200 mL), EBC sample pH of 10.0 and centrifugation at 6000 rpm for 5 minutes. The conditions for ULLME were 150 mL of chloroform and the samples were sonicated for 4 minutes. The method was validated over the concentration range of 0.5–10 mg/L-1 in EBC. Inter- and intra-day precision and accuracy were less than 5 % where the acceptable levels are less than 20%.  Furthermore, the validated method was successfully applied for the determination of methadone in patients’ EBC samples. Conclusions. The outcomes indicate that the developed LC-UV combined with DLLME and/or ULLME extraction methods can be employed for the extraction and separation of methadone in EBC samples. This article is open to POST-PUBLICATION REVIEW. Registered readers (see “For Readers”) may comment by clicking on ABSTRACT on the issue’s contents page.


2019 ◽  
Vol 15 (5) ◽  
pp. 535-541 ◽  
Author(s):  
Fariba Pourkarim ◽  
Ali Shayanfar ◽  
Maryam Khoubnasabjafari ◽  
Fariborz Akbarzadeh ◽  
Sanaz Sajedi-Amin ◽  
...  

Background:Developing a simple analysis method for quantification of drug concentration is one of the essential issues in pharmacokinetic and therapeutic drug monitoring studies.Objective:A fast and reliable dispersive liquid-liquid microextraction procedure was employed for preconcentration of verapamil in exhaled breath condensate (EBC) samples and this was followed by the determination with high-performance liquid chromatography-ultraviolet detection.Methods:A reverse-phase high-performance liquid chromatography (RP-HPLC) combined with a dispersive liquid-liquid microextraction method (DLLME) was applied for quantification of verapamil in the EBC samples. The developed method was validated according to FDA guidelines.Results:Under the optimum conditions, the method provided a linear range between 0.07 and 0.8 µg.mL-1 with a coefficient of determination of 0.998. The intra- and inter-day relative standard deviation and relative error values of the method were below 15%, which indicated good precision and accuracy. The proposed method was successfully applied for the analysis of verapamil in two real samples with concentrations of 0.07 and 0.09 µg.mL-1.Conclusion:The established HPLC-UV-DLLME method could be applied for the analysis of verapamil in human EBC samples.


2020 ◽  
Vol 16 (7) ◽  
pp. 872-879
Author(s):  
Samin Hamidi

Background: Abuse of drugs is associated with several medical, forensic, toxicology and social challenges. “Drugs of abuse” testing is therefore an important issue. Objective: We propose a simple CE-based method for the quantification of amphetamine, codeine and morphine after direct injection of Exhaled Breath Condensate (EBC) by the aid of simple stacking mode and an off-line pre-concentration method. Methods: Using graphene oxide adsorbents, amphetamine, codeine and morphine were extracted from EBC in order to eliminate the proteins and other interferences. In addition to off-line method, an online stacking mode was applied to improve the analytical signal obtained from the instrument. Results: The validation parameters were experimented on the developed method based on the FDA guideline over concentration ranges of 12.5-100, 30-500 and 10-1250 ng/mL associated with amphetamine, codeine and morphine, respectively. Small volumes (around 100 μL) of EBC were collected using a lab-made setup and successfully analyzed using the proposed method where precisions and accuracies (within day and between days) were in accordance with the guideline (recommended less than 15 % for biological samples). The recovery tests were used to evaluate the matrix effect and data (94 to 105 %) showed that the proposed method can be applied in different EBC matrix samplings of subjects. Conclusion: The proposed method is superior for simultaneous determination of amphetamine, codeine and morphine over chromatographic analyses because it is fast and consumes fewer chemicals, with no derivatization step.


2021 ◽  
Author(s):  
Fariba Pourkarim ◽  
Elaheh Rahimpour ◽  
Maryam Khoubnasabjafari ◽  
Vahid Jouyban-Gharamaleki ◽  
Afshin Gharakhani ◽  
...  

2018 ◽  
Vol 126 ◽  
pp. 334-340 ◽  
Author(s):  
Joshua D. Chandler ◽  
Hamed Horati ◽  
Douglas I. Walker ◽  
Enea Pagliano ◽  
Rabindra Tirouvanziam ◽  
...  

2016 ◽  
Vol 31 (4) ◽  
pp. 924-933 ◽  
Author(s):  
Elizabeth Leese ◽  
Jackie Morton ◽  
Philip H. E. Gardiner ◽  
Vikki A. Carolan

A method development study describing the first simultaneous determination of Cr(III) and Cr(VI) in an exhaled breath condensate sample.


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