title: Evaluation of sequential injection chromatography for reversed phase separation of triazine herbicides exploiting monolithic and core-shell columns.
abstract: This paper describes the development of reversed phase sequential injection chromatography (SIC) methods for separation of simazine (SIM) and atrazine (AT), as well as their metabolites deethylatrazine (DEA), deisopropylatrazine (DIA) and hydroxyatrazine (HAT) exploiting silica based monolithic (50 × 4.6 mm) and core-shell (30 × 4.6 mm, 2.7 µm particles) columns. The separation was made by stepwise elution with two mobile phases: MP1 composed of 15:85 (v/v) acetonitrile: 2.5 mmol L(-1) acetic acid/ammonium acetate buffer (pH 4.2), and MP2, composed of 35:65 (v/v) acetonitrile: 2.5 mmol L(-1) acetic acid/ammonium acetate buffer (pH 4.2).The less hydrophobic compounds (DIA, HAT and DEA) eluted with MP1, whereas SIM and AT eluted with MP2. The method using core-shell column exhibited better chromatographic efficiency compared with monolithic column for separation of SIM and AT, but failed to provide base line separation of DIA and HAT. The proposed composition of mobile phases enabled the monolithic column to separate all the studied compounds with resolution >2.3 at flow rate of 35 µL s(-1) and sampling throughput of 8 analyses per hour, whereas in the core-shell the maximum flow rate allowed in the SIC system was 8 µL s(-1) (sampling throughput of 3 analyses per hour). The limits of detection were between 24 µg L(-1) (AT) and 40 µg L(-1) (DEA) using the monolithic column, and between 20 µg L(-1) (SIM) and 38 µg L(-1) (DEA) with the core-shell. Ultrasound-assisted extraction (80:20 v/v acetonitrile:water) of a soil sample enriched with the five triazines (250, 500 and 1000 µg kg(-1)) resulted recoveries between 51% and 121% of the spiked concentrations.
authors.affiliation: Instituto de Química, Universidade de São Paulo, C.P. 26077, 05513-970 São Paulo, SP, Brazil.
authors.forename: Ricardo
authors.initials: R
authors.lastname: de Prá Urio
authors.affiliation: Instituto de Química, Universidade de São Paulo, C.P. 26077, 05513-970 São Paulo, SP, Brazil. Electronic address: jcmasini@iq.usp.br.
authors.forename: Jorge C
authors.initials: JC
authors.lastname: Masini
mesh_terms: D000097:Acetonitriles / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation / Q000379:methods*; D056148:Chromatography, Reverse-Phase / Q000295:instrumentation / Q000379:methods*; D017022:Flow Injection Analysis / Q000295:instrumentation / Q000379:methods*; D006540:Herbicides / Q000032:analysis / Q000302:isolation & purification*; D012989:Soil Pollutants / Q000737:chemistry*; D014227:Triazines / Q000032:analysis / Q000302:isolation & purification*
chemical_list: D000097:Acetonitriles; D006540:Herbicides; D012989:Soil Pollutants; D014227:Triazines; C032159:acetonitrile
keywords: Atrazine; Metabolites; Sequential injection; Simazine; Soil