Determination of Parabens in Surface Water from Mogi Guaçu River (São Paulo, Brazil) Using Dispersive Liquid-Liquid Microextraction Based on Low Density Solvent and LC-DAD

Galinaro, Carlos A.; Pereira, Fabiana M.; Vieira, Eny M.

doi:10.5935/0103-5053.20150206

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Articles • J. Braz. Chem. Soc. 26 (11) • Nov 2015 • https://doi.org/10.5935/0103-5053.20150206 copy

Determination of Parabens in Surface Water from Mogi Guaçu River (São Paulo, Brazil) Using Dispersive Liquid-Liquid Microextraction Based on Low Density Solvent and LC-DAD

Authorship SCIMAGO INSTITUTIONS RANKINGS

A method using dispersive liquid-liquid microextraction (DLLME) based on low density solvent (LDS) combined with liquid chromatography with diode array detection (LC-DAD) has been developed for determination of parabens. Some DLLME parameters such as kind and volumes of extraction and disperser solvents, pH of the aqueous samples, ionic strength, extraction, centrifugation and speed time, were investigated. The method exhibits good linearity (0.9990 to 0.9993), limits of detection (0.5-0.8 µg L^-1), and limits of quantification (1.3-2.4 µg L^-1). In optimum conditions, enrichment factors and recoveries of studied parabens obtained were 38.9 to 88.4% and 30.3 to 68.0%, respectively. Surface water samples collected from Mogi Guaçu River (São Paulo state, Brazil) were analyzed, showing average contents of methyl-, ethyl-, propyl-, and n-butylparaben of 8.0, 5.8, 13.1 and 15.1 µg L^-1, respectively. This is the first study on parabens in a Brazilian River, in a long stretch of river (ca. 300 km of extension).

Keywords:
dispersive liquid-liquid microextraction; low density solvent; Mogi Guaçu River; paraben; sample preparation

Compound	LR^a a LR = linear range; / (μg L^-1)	R²^b b R2 = square of correlation coefficient;	LOD^c c LOD = limit of detection (S/N = 3); / (μg L^-1)	LOQ^d d LOQ = limit of quantification (S/N = 10); / (μg L^-1)	RSD^e e RSD = relative standard deviation (C = 50 μg L-1, n = 3); / %	EF^f f EF = enrichment factor; ± SD^g g SD = standard deviation;	ER^h h ER = extraction recovery. ±SD^g g SD = standard deviation; / %
Methylparaben	1-50	0.9992	0.8	2.4	8.3	38.9 ± 5.2	30.3 ± 3.9
Ethylparaben	1-50	0.9993	0.8	1.9	8.1	72.1 ± 13.8	56.6 ± 12.9
Propylparaben	1-50	0.9990	0.5	1.3	6.7	88.4 ± 9.9	68.0 ± 7.6
Butylparaben	1-50	0.9990	0.8	2.0	6.3	50.7 ± 8.9	41.1 ± 7.7

Method	Compound	LOD^a a LOD = limit of detection; / (µg L^-1)	LOQ^b b LOQ = limit of quantification; / (µg L^-1)	Sample amount / mL	Recovery / %	EF^c c EF = enrichment factor;	Extraction time / min	Reference
DLLME/GC-FID^d d dispersive liquid-liquid microextraction combined with gas chromatography-flame ionization detection;	methylparaben	15	50	10	25	100	10	18
	ethylparaben	5	20		52	202
	propylparaben	5	20		72	276
DLLME/LC-UV^e e dispersive liquid-liquid microextraction combined with liquid chromatography with ultraviolet detection;	methylparaben	0.046	0.15	5	25	27	1	4
	ethylparaben	0.043	0.14		48	50
	propylparaben	0.022	0.07		67	70
	butylparaben	0.021	0.07		86	90
SPE/GC-MS^f f solid phase extraction combined with gas chromatography-mass spectrometry;	methylparaben	0.0005	−	1000	81.1	−	−	14
	ethylparaben	0.0006	−		90.9	−
	propylparaben	0.0005	−		91.2	−
	butylparaben	0.0006	−		97.6	−
SFC-HS-SPME-GC-MS^g f solid phase extraction combined with gas chromatography-mass spectrometry;	methylparaben	0.5	1.7	−	97.6	−	15	19
	ethylparaben	2.0	6.6		90.6	−
	propylparaben	8.3	27.5		91.2	−
	butylparaben	8.3	27.7		99.6	−
SPME-GC-MS^h g supercritical fluid extraction on-line headspace solid-phase microextraction combined with gas chromatography-mass spectrometry;	methylparaben	0.00170	−	10	86	−	12	22
	ethylparaben	0.00088	−		91	−
	propylparaben	0.00040	−		85	−
	butylparaben	0.00057	−		88	−
SBSE/GC-MSⁱ h solid phase extraction combined with gas chromatography-mass spectrometry;	methylparaben	1.06	3.22	−	102	−	240	23
	propylparaben	0.74	1.56		110	−
	butylparaben	0.08	2.26		104	−
DLLME-LDS/DAD^j i stir-bar sorptive extraction combined with gas chromatography-mass spectrometry;	methylparaben	0.8	2.4	5	30.3	38.9	2	this work
	ethylparaben	0.8	1.9		56.6	72.1
	propylparaben	0.5	1.3		68.0	88.4
	butylparaben	0.8	2.0		41.1	51.7

City (Site)	MP^a a Methylparaben; ± SD^b b SD: standard deviation (n = 3); /(μg L^-1)	EP^c c ethylparaben; ± SD^b b SD: standard deviation (n = 3); /(μg L^-1)	PP^d d propylparaben; ± SD^b b SD: standard deviation (n = 3); /(μg L^-1)	BP^e e butylparaben; ± SD^b b SD: standard deviation (n = 3); /(μg L^-1)	Total parabens ± SD^b b SD: standard deviation (n = 3); /(μg L^-1)
Guatapará (1)	< LOD^f f LOD = limit of detection (S/N = 3);	6.1 ± 0.5	1.6 ± 0.1	13.0 ± 0.8	20.7 ± 1.4
Rincão (2)	3.0 ± 0.3	2.1 ± 0.5	3.2 ± 0.2	< LOD^f f LOD = limit of detection (S/N = 3);	8.3 ± 1.0
Porto Ferreira (3)	2.5 ± 0.2	2.3 ± 0.2	18.3 ± 1.2	< LOD^f f LOD = limit of detection (S/N = 3);	23.1 ± 1.6
Porto Ferreira (4)	< LOQ^g g LOQ = limit of quantification (S/N = 10);	2.6 ± 0.2	< LOQ^g g LOQ = limit of quantification (S/N = 10);	< LOD^f f LOD = limit of detection (S/N = 3);	2.6 ± 0.2
Cachoeira de Emas (5)	2.7 ± 0.2	2.0 ± 0.2	1.4 ± 0.1	17.7 ± 1.1	23.8 ± 1.7
Cachoeira de Emas (6)	9.4 ± 0.8	< LOD^f f LOD = limit of detection (S/N = 3);	2.0 ± 0.2	< LOD^f f LOD = limit of detection (S/N = 3);	11.4 ± 1.0
Pirassununga (7)	< LOD^f f LOD = limit of detection (S/N = 3);	< LOD^f f LOD = limit of detection (S/N = 3);	45.6 ± 3.1	< LOD^f f LOD = limit of detection (S/N = 3);	45.6 ± 3.1
Martinho Prado (8)	< LOD^f f LOD = limit of detection (S/N = 3);	2.4 ± 0.2	< LOQ^g g LOQ = limit of quantification (S/N = 10);	9.3 ± 0.6	11.7 ± 0.8
Mogi Guaçu (9)	< LOD^f f LOD = limit of detection (S/N = 3);	< LOQ^g g LOQ = limit of quantification (S/N = 10);	< LOD^f f LOD = limit of detection (S/N = 3);	19.9 ± 1.3	19.9 ± 1.3
Mogi Guaçu (10)	27.5 ± 2.3	30.5 ± 2.5	2.8 ± 0.2	< LOQ^g g LOQ = limit of quantification (S/N = 10);	60.8 ± 5.0
Mogi Guaçu (11)	ND^h h ND = not detected.	< LOQ^g g LOQ = limit of quantification (S/N = 10);	2.1 ± 0.2	< LOQ^g g LOQ = limit of quantification (S/N = 10);	2.1 ± 0.2
Mogi Guaçu (12)	< LOD^f f LOD = limit of detection (S/N = 3);	1.9 ± 0.2	1.7 ± 0.1	15.5 ± 1.0	19.1 ± 1.3
Mogi Guaçu (13)	2.6 ± 0.2	2.2 ± 0.2	52.1 ± 3.5	< LODf	56.9 ± 3.9
Itapira (14)	< LOD^f f LOD = limit of detection (S/N = 3);	< LOD^f f LOD = limit of detection (S/N = 3);	< LOD^f f LOD = limit of detection (S/N = 3);	< LOD^f f LOD = limit of detection (S/N = 3);	< LOD^f f LOD = limit of detection (S/N = 3);
Average	8.0 ± 0.7	5.8 ± 0.5	13.1 ± 0.9	15.1 ± 0.9	−

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