Automated online coupling of robot-assisted single drop microextraction and liquid chromatography

Author(s)

Vargas Medina, Deyber Arley ^[1] ; Rodriguez Cabal, Luis Felipe ^[1] ; Titato, Guilherme Miola ^[1] ; Lancas, Fernando Mauro ^[1] ; Santos-Neto, Alvaro Jose ^[1]

Affiliation

^[1] Univ Sao Paulo, Sao Carlos Inst Chem, BR-13566590 Sao Carlos, SP - Brazil

• Document type: Journal article
• Source: Journal of Chromatography A; v. 1595, p. 66-72, JUN 21 2019.
• Web of Science Citations: 5

Abstract

A high-throughput and innovative setup has been developed to automate the online integration of single drop microextraction (SDME), liquid chromatography (LC) and high-resolution mass spectrometry (QqToF). SDME and LC were online hyphenated for the first time. SDME was carried out by a lab-made cartesian robot actuating a 100 mu L syringe, equipped with a three-way solenoid microvalve that allowed the online transference of the enriched extract to the chromatographic system, through a six-port switching valve. The complete method, including the synchronized robot action, valves, and the analytical instruments, was controlled by an Arduino Mega board. The merits of the proposed setup were demonstrated by the triazines determination in coconut water samples. The most relevant extraction parameters, such as drop size, exposure time, stirring effect, salt addition and pH were systematically investigated. Under optimized conditions (60 mu L drop volume and 10 min extraction time), the LC-UV enrichment factors (EF) and the extraction recoveries (ER) ranged between 15.2-18.4 and 11.4-13.8%, respectively. Using the SDME-LC-MS setup, the linear range, detection limit (S/N = 3) and precision (RSD, n = 6 at 0.25 mu g L-1 level of concentration) were 0.25-25 mu g L-1, 0.10 mu g L-1 and 16.8% for simazine; 0.25-25 mu g L-1, 0.05 mu g L-1 and 14.7% for atrazine; and 0.25-25 mu g L-1, 0.05 mu g L-1 and 18.5% for propazine, respectively. Although none of the analytes were detected in the evaluated commercial samples, the results indicate that the proposed online SDME-LC setup is a competitive analytical strategy for the determination of target organic compounds in complex matrices. (C) 2019 Elsevier B.V. All rights reserved. (AU)

• FAPESP's process: 17/02147-0 - Single drop chromatography and its coupling to mass spectrometry: instrumental strategies, development of materials, automation and analytical applications
• Grantee: Fernando Mauro Lanças
• Support Opportunities: Research Projects - Thematic Grants
• FAPESP's process: 10/19910-9 - Development of green chemistry strategies on chromatography and application to the evaluation of antibiotics degradation in wastewaters by fixed-bed anaerobic bioreactors
• Grantee: Alvaro José dos Santos Neto
• Support Opportunities: Regular Research Grants
• FAPESP's process: 16/21950-5 - Automation strategies for miniaturized sample preparation, case: automated online in syringe stirred SDME
• Grantee: Deyber Arley Vargas Medina
• Support Opportunities: Scholarships abroad - Research Internship - Doctorate