An automated in-syringe switchable hydrophilicity solvent-based microextraction

Research output

Abstract

A fully automated in-syringe switchable hydrophilicity solvent-based microextraction approach was suggested for the first time. Di-(2-ethylhexyl)phosphoric acid was investigated as a novel switchable hydrophilicity solvent. The microextraction procedure implemented into a syringe pump included dissociation of the extractant in alkaline sample solution resulting in homogeneous solution formation followed by in situ organic phase generation by acidification and its separation. The microextraction procedure was applied to the HPLC-UV determination of antimicrobial drugs (sulfamethoxazole and sulfamethazine) in human urine samples as a proof-of-concept example. The calibration graphs were linear over the concentration ranges of 0.06–50 mg L−1 for sulfamethoxazole and 0.13–50 mg L−1 for sulfamethazine. The LODs calculated from the blank tests based on 3σ were 0.02 and 0.04 mg L−1 for sulfamethoxazole and sulfamethazine, respectively. The sample throughput was 12 samples h−1. The possibility of using the proposed procedure for assessing sulfamethoxazole/sulfamethazine acetylation in metabolic processes by individual human phenotypes was shown.
Original languageEnglish
JournalTalanta
Volume209
Issue number1
Early online date24 Nov 2019
Publication statusPublished - 2020

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Sulfamethazine
Sulfamethoxazole
Syringes
Hydrophilicity
Acetylation
Acidification
Throughput
Pumps
Calibration
Pharmaceutical Preparations

Cite this

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title = "An automated in-syringe switchable hydrophilicity solvent-based microextraction",
abstract = "A fully automated in-syringe switchable hydrophilicity solvent-based microextraction approach was suggested for the first time. Di-(2-ethylhexyl)phosphoric acid was investigated as a novel switchable hydrophilicity solvent. The microextraction procedure implemented into a syringe pump included dissociation of the extractant in alkaline sample solution resulting in homogeneous solution formation followed by in situ organic phase generation by acidification and its separation. The microextraction procedure was applied to the HPLC-UV determination of antimicrobial drugs (sulfamethoxazole and sulfamethazine) in human urine samples as a proof-of-concept example. The calibration graphs were linear over the concentration ranges of 0.06–50 mg L−1 for sulfamethoxazole and 0.13–50 mg L−1 for sulfamethazine. The LODs calculated from the blank tests based on 3σ were 0.02 and 0.04 mg L−1 for sulfamethoxazole and sulfamethazine, respectively. The sample throughput was 12 samples h−1. The possibility of using the proposed procedure for assessing sulfamethoxazole/sulfamethazine acetylation in metabolic processes by individual human phenotypes was shown.",
keywords = "Automated in-syringe switchable hydrophilicity solvent-based microextraction, Flow analysis, High performance liquid chromatography with ultraviolet detection, Acetylation phenotype, SULFONAMIDE, Human urine",
author = "Aleksei Pochivalov and Christina Vakh and Sergei Garmonov and Leonid Moskvin and Andrey Bulatov",
year = "2020",
language = "English",
volume = "209",
journal = "Talanta",
issn = "0039-9140",
publisher = "Elsevier",
number = "1",

}

TY - JOUR

T1 - An automated in-syringe switchable hydrophilicity solvent-based microextraction

AU - Pochivalov, Aleksei

AU - Vakh, Christina

AU - Garmonov, Sergei

AU - Moskvin, Leonid

AU - Bulatov, Andrey

PY - 2020

Y1 - 2020

N2 - A fully automated in-syringe switchable hydrophilicity solvent-based microextraction approach was suggested for the first time. Di-(2-ethylhexyl)phosphoric acid was investigated as a novel switchable hydrophilicity solvent. The microextraction procedure implemented into a syringe pump included dissociation of the extractant in alkaline sample solution resulting in homogeneous solution formation followed by in situ organic phase generation by acidification and its separation. The microextraction procedure was applied to the HPLC-UV determination of antimicrobial drugs (sulfamethoxazole and sulfamethazine) in human urine samples as a proof-of-concept example. The calibration graphs were linear over the concentration ranges of 0.06–50 mg L−1 for sulfamethoxazole and 0.13–50 mg L−1 for sulfamethazine. The LODs calculated from the blank tests based on 3σ were 0.02 and 0.04 mg L−1 for sulfamethoxazole and sulfamethazine, respectively. The sample throughput was 12 samples h−1. The possibility of using the proposed procedure for assessing sulfamethoxazole/sulfamethazine acetylation in metabolic processes by individual human phenotypes was shown.

AB - A fully automated in-syringe switchable hydrophilicity solvent-based microextraction approach was suggested for the first time. Di-(2-ethylhexyl)phosphoric acid was investigated as a novel switchable hydrophilicity solvent. The microextraction procedure implemented into a syringe pump included dissociation of the extractant in alkaline sample solution resulting in homogeneous solution formation followed by in situ organic phase generation by acidification and its separation. The microextraction procedure was applied to the HPLC-UV determination of antimicrobial drugs (sulfamethoxazole and sulfamethazine) in human urine samples as a proof-of-concept example. The calibration graphs were linear over the concentration ranges of 0.06–50 mg L−1 for sulfamethoxazole and 0.13–50 mg L−1 for sulfamethazine. The LODs calculated from the blank tests based on 3σ were 0.02 and 0.04 mg L−1 for sulfamethoxazole and sulfamethazine, respectively. The sample throughput was 12 samples h−1. The possibility of using the proposed procedure for assessing sulfamethoxazole/sulfamethazine acetylation in metabolic processes by individual human phenotypes was shown.

KW - Automated in-syringe switchable hydrophilicity solvent-based microextraction

KW - Flow analysis

KW - High performance liquid chromatography with ultraviolet detection

KW - Acetylation phenotype

KW - SULFONAMIDE

KW - Human urine

UR - https://www.sciencedirect.com/science/article/pii/S0039914019312202

UR - https://www.ncbi.nlm.nih.gov/pubmed/31892021

M3 - Article

VL - 209

JO - Talanta

JF - Talanta

SN - 0039-9140

IS - 1

ER -