TY - JOUR
T1 - Factorial design optimisation of solid phase extraction for preconcentration of parabens in wastewater using ultra-high performance liquid chromatography triple quadrupole mass spectrometry
AU - Muckoya, Vallerie A.
AU - Nomngongo, Philiswa N.
AU - Ngila, Jane C.
N1 - Publisher Copyright:
© 2020 Bentham Science Publishers.
PY - 2020
Y1 - 2020
N2 - Background: Parabens are synthetic esters used extensively as preservatives and/or bactericides in personal care personal products. Objective: Development and validation of a novel robust chemometric assisted analytical technique with superior analytical performances for the determination of ethylparaben, methylparaben and propylparaben, using simulated wastewater matrix. Methods: An automated Solid Phase Extraction (SPE) method coupled with liquid chromatographymass spectrometry was applied in this study. A gradient elution programme comprising of 0.1% formic acid in deionised water (A) and 0.1% formic acid in Methanol (B) was employed on a 100 x 2.1 mm, 3.0 µm a particle size biphenyl column. Two-level (2k) full factorial design coupled with response surface methodology was used for optimisation and investigation of SPE experimental variables that had the most significant outcome of the analytical response. Results: According to the analysis of variance (ANOVA), sample pH and eluent volume were statistically the most significant parameters. The method developed was validated for accuracy, precision, Limits of Detection (LOD) and Limit of Quantification (LOQ) and linearity. The LOD and LOQ established under those optimised conditions varied between 0.04-0.12 µgL-1 and 0.14-0.40 µgL-1 respectively. The use of matrix-matched external calibration provided extraction recoveries between 78-128% with relative standard deviations at 2-11% for two spike levels (10 and 100 µgL-1) in three different water matrices (simulated wastewater, influent and effluent water). Conclusion: The newly developed method was applied successfully to the analyses of parabens in wastewater samples at different sampling points of a wastewater treatment plant, revealing concentrations of up to 3 µgL-1.
AB - Background: Parabens are synthetic esters used extensively as preservatives and/or bactericides in personal care personal products. Objective: Development and validation of a novel robust chemometric assisted analytical technique with superior analytical performances for the determination of ethylparaben, methylparaben and propylparaben, using simulated wastewater matrix. Methods: An automated Solid Phase Extraction (SPE) method coupled with liquid chromatographymass spectrometry was applied in this study. A gradient elution programme comprising of 0.1% formic acid in deionised water (A) and 0.1% formic acid in Methanol (B) was employed on a 100 x 2.1 mm, 3.0 µm a particle size biphenyl column. Two-level (2k) full factorial design coupled with response surface methodology was used for optimisation and investigation of SPE experimental variables that had the most significant outcome of the analytical response. Results: According to the analysis of variance (ANOVA), sample pH and eluent volume were statistically the most significant parameters. The method developed was validated for accuracy, precision, Limits of Detection (LOD) and Limit of Quantification (LOQ) and linearity. The LOD and LOQ established under those optimised conditions varied between 0.04-0.12 µgL-1 and 0.14-0.40 µgL-1 respectively. The use of matrix-matched external calibration provided extraction recoveries between 78-128% with relative standard deviations at 2-11% for two spike levels (10 and 100 µgL-1) in three different water matrices (simulated wastewater, influent and effluent water). Conclusion: The newly developed method was applied successfully to the analyses of parabens in wastewater samples at different sampling points of a wastewater treatment plant, revealing concentrations of up to 3 µgL-1.
KW - Ethylparaben
KW - Factorial design
KW - Methylparaben
KW - Propylparaben
KW - Solid phase extraction
KW - UHPLC-MS/MS
KW - Wastewater
UR - http://www.scopus.com/inward/record.url?scp=85086341697&partnerID=8YFLogxK
U2 - 10.2174/1573411014666180627150854
DO - 10.2174/1573411014666180627150854
M3 - Article
AN - SCOPUS:85086341697
SN - 1573-4110
VL - 16
SP - 436
EP - 446
JO - Current Analytical Chemistry
JF - Current Analytical Chemistry
IS - 4
ER -