scholarly journals MEASUREMENT OF CORTISOL IN HUMAN PLASMA AND URINE BY ULTRA PERFORMANCE LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY

Author(s):  
Syed N Alvi ◽  
Muhammad M Hammami

Objective: The objective of this study is to develop and validate a simple, sensitive, specific, and rapid assay for quantification of clinically relevant cortisol level in human plasma and urine samples.Methods: Ultra performance liquid chromatographic-tandem mass spectrometric (UPLC-MS/MS) analysis was performed on Atlantis dC18 column (2.1×100 mm, 3 μm) with a mobile phase consisting of acetonitrile and 2 mM ammonium acetate (50:50, v: v) that was delivered at a flow rate of 0.3 ml/min. Tolperisone (2 ng) was used as an internal standard (IS). Biological samples were extracted with a mixture of hexane and methyl tert-butyl ether (8:2, v: v). The eluents were monitored using electrospray ionization in the positive ion mode with transition mass to charge ratio set at 363.1 → 121.0 and 246.0 → 97.9 for cortisol and IS, respectively. The method was validated according to international guidelines.Results: Retention times of cortisol and IS were about 1.4 and 2.3, respectively. Relationship between cortisol level and peak area ratio of cortisol to IS was linear (R2≥0.987) in the range of 2.5–400 ng/ml and 1.0–200 ng/ml in plasma and urine samples, respectively. Intra- and inter-day coefficient of variation and bias were ≤9.7% and ±11.1%, and ≤10.4% and ±11.5% for plasma and urine samples, respectively. Extraction recoveries were in 80–91% for cortisol plasma and 80–86% for cortisol in urine samples. Cortisol was ≥86% stable when stored at room temperature for 24 h or at −20°C for 24 weeks in plasma samples and ≥93% stable when stored at room temperature for 24 h or −20°C for 16 weeks in urine samples.Conclusion: We report a validated, clinically relevant, simple, and rapid UPLC-MS/MS assay of cortisol level in human plasma and urine.

RSC Advances ◽  
2015 ◽  
Vol 5 (129) ◽  
pp. 106574-106588 ◽  
Author(s):  
Behruz Barfi ◽  
Alireza Asghari ◽  
Maryam Rajabi ◽  
Nasim Mirkhani

A dispersive suspended-solidified floating organic droplet microextraction method was developed for determination of some nonsteroidal anti-inflammatory drugs in human plasma and urine samples.


Molecules ◽  
2020 ◽  
Vol 25 (24) ◽  
pp. 5799
Author(s):  
Olga Maliszewska ◽  
Natalia Treder ◽  
IIona Olędzka ◽  
Piotr Kowalski ◽  
Natalia Miękus ◽  
...  

A new approach for the sensitive, robust and rapid determination of idarubicin (IDA) in human plasma and urine samples based on liquid chromatography with fluorescence detection (LC-FL) was developed. Satisfactory chromatographic separation of the analyte after solid-phase extraction (SPE) was performed on a Discovery HS C18 analytical column using a mixture of acetonitrile and 0.1% formic acid in water as the mobile phase in isocratic mode. IDA and daunorubicin hydrochloride used as an internal standard (I.S.) were monitored at the excitation and emission wavelengths of 487 and 547 nm, respectively. The method was validated according to the FDA and ICH guidelines. The linearity was confirmed in the range of 0.1–50 ng/mL and 0.25–200 ng/mL, while the limit of detection (LOD) was 0.05 and 0.125 ng/mL in plasma and urine samples, respectively. The developed LC-FL method was successfully applied for drug determinations in human plasma and urine after oral administration of IDA at a dose of 10 mg to a patient with highly advanced alveolar rhabdomyosarcoma (RMA). Moreover, the potential exposure to IDA present in both fluids for healthcare workers and the caregivers of patients has been evaluated. The present LC-FL method can be a useful tool in pharmacokinetic and clinical investigations, in the monitoring of chemotherapy containing IDA, as well as for sensitive and reliable IDA quantitation in biological fluids.


2015 ◽  
Vol 27 (12) ◽  
pp. 4615-4619 ◽  
Author(s):  
D. Mahaboob Basha ◽  
G. Venkata Reddy ◽  
T. Shobha Rani ◽  
E. Susithra ◽  
Rajasekhar Chekkara

2019 ◽  
Vol 3 (Supplement_1) ◽  
Author(s):  
Amandeep Sandhu ◽  
Jiayi Fan ◽  
Di Xiao ◽  
Indika Edirisinghe ◽  
Britt Burton-Freeman

Abstract Objectives Mango contains considerable amounts of phytochemicals, most notably phenolic acids, mangiferin, carotenoids and gallotannins. However, little is known how these compounds are metabolized in the human body. The objective of this study was to identify the phenolic metabolites in human plasma and urine after mango consumption. Methods Blood and urine samples were collected at baseline (t = 0 h) and then at 2 h, 8 h, 24 h after mango pulp (500 g) consumption by healthy adults. Pooled plasma and urine samples at different time-points (n = 12; age 30.0 ± 7.6 y and BMI 22.4 ± 1.7 kg/m2) were extracted using solid phase extraction procedure. Phytochemicals in mango pulp were extracted using extraction solution (acetone: water: acetic acid = 70: 29.7: 0.3 v/v). Compounds were identified and quantified using Ultra High Performance Liquid Chromatography (UHPLC) system coupled to iFunnel Quadrupole Time of Flight mass spectrometer (MS) and UHPLC system with Triple Quadrupole MS, respectively. Separation of compounds was achieved by reversed phase chromatography and compounds were identified based on mass accuracy (< 5 ppm), specific fragmentation pattern, previous literature reports and co-chromatography when standards were available. Results A total of 31 compounds were tentatively identified and quantified in the mango pulp, including mangiferin (16.48 ± 1.13 µg/100 g fresh weight (FW)), catechin (24.50 ± 8.46 µg/100 g FW), and total gallic acid (2024.2 ± 83.8 mg/100 g FW). A total of 59 and 164 phenolic metabolites were tentatively identified at different time-points in plasma and urine, respectively. The compounds detected in 2 h plasma and urine samples were mostly small phenolic acids such as hippuric acid, cinnamic acid, abscisic acid, gallic acid along with their methyl and glucuronide conjugates. Other compounds such as pyrogalloyl sulfate, methyl and glucuronide conjugates, cinnamic acid, phenylacetic acid and benzoic acid derivatives appeared post 8 and 24 h consumption of mango pulp. Conclusions Our results suggest that mango polyphenols are absorbed and extensively metabolized resulting in the production of various phenolic metabolites and their conjugates, all together contributing to the bioavailability and potential health benefits associated with mango consumption. Funding Sources National Mango Board.


2020 ◽  
Vol 34 (10) ◽  
Author(s):  
Sezin Erarpat ◽  
Süleyman Bodur ◽  
Merve Fırat Ayyıldız ◽  
Ömer Tahir Günkara ◽  
Fatih Erulaş ◽  
...  

Sign in / Sign up

Export Citation Format

Share Document