Polyvinyl Alcohol/Pectin-Based Hydrogel as Sorptive Phase for the Determination of Freely Dissolved Parabens in Urine Samples by LC-DAD

Marinho, Andressa; Silva, Bruno José G. da

doi:10.21577/0103-5053.20230093

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Journal of the Brazilian Chemical Society

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Article • J. Braz. Chem. Soc. 34 (11) • 2023 • https://doi.org/10.21577/0103-5053.20230093 copy

Polyvinyl Alcohol/Pectin-Based Hydrogel as Sorptive Phase for the Determination of Freely Dissolved Parabens in Urine Samples by LC-DAD

Authorship SCIMAGO INSTITUTIONS RANKINGS

An extraction phase based on hydrogel disks of polyvinyl alcohol and pectin was developed, characterized, and evaluated for the extraction of four endocrine disruptors (methylparaben, ethylparaben, propylparaben and butylparaben) in free form in human urine samples with subsequent determination by liquid chromatography coupled with a diode array detector (LC-DAD). The proposed hydrogel showed easy synthesis, was made of low-cost and non-toxic polymers, and showed that it has an amphiphilic character. Gels with lower swelling indexes (175%) and more concentrated dispersions of polymers (P20PC2.0) showed lower relative standard deviation (RSD) values. Under optimized solid phase extraction (SPE) conditions, the LC-DAD method presented limits of quantification of 0.1 µg mL¹, accuracy values ranged from 101.3 to 118.2%, while the inter-assay precision ranged from 1.5 to 17.4%. In addition, the polyvinyl alcohol (PVOH)/pectin-based material presented the possibility of reuse at least 15 times, without presenting carryover effect and physical degradation. In this way, the hydrogel shows promise for the extraction of organic compounds with different polarities in biological matrices.

Keywords:
hydrogel; polyvinyl alcohol; pectin; human urine; parabens; solid phase extraction

Analyte	Equation of straight line $(y = ax + b)$	Standard errors	R²	LLOQ			LOD / (µg mL 1)
Analyte	Equation of straight line $(y = ax + b)$	a/b	R²	Concentration / (µg mL^-1)	RSD / %	Accuracy / %	LOD / (µg mL 1)
MPB	$y = 0.49627 x - 0.02629$	0.021/0.009	0.9926	0.1	17.4	118.2	0.034
EPB	$y = 0.63600 x - 0.02141$	0.022/0.006	0.9951	0.1	12.1	109.8	0.020
PPB	$y = 0.96275 x + 0.01072$	0.009/0.004	0.9996	0.1	6.4	101.7	0.007
BPB	$y = 1.24171 x + 0.02220$	0.017/0.003	0.9992	0.1	3.8	101.3	0.005

Analyte	Concentration / (µg mL^-1)	RSD / %	Accuracy / %
MPB	0.1	17.4	118.2
	0.5	10.1	108.0
	1.0	6.4	102.1
EPB	0.1	12.1	109.8
	0.5	14.2	103.3
	1.0	3.4	102.8
PPB	0.1	6.4	101.7
	0.5	1.5	99.8
	1.0	9.0	96.6
BPB	0.1	3.8	101.3
	0.5	5.0	99.5
	1.0	6.8	98.8

Sample preparation	Analytical technique	Pre-treatment urine	LLOQ / (µg mL^-1)	LOD / (µg mL^-1)	Reference
DLLME	cLC-UV	enzymatic hydrolysis	0.023-0.036	0.007-0.011	48
FPSE	LC-DAD	-	0.01	0.003	38
FPSE	LC-DAD	-	0.1	0.03	37
MEPS	LC-MS/MS	enzymatic hydrolysis	0.00005-0.00033	0.0001	49
SPE	UPLC-MS/MS	enzymatic hydrolysis	0.0003-0.001	0.00009-0.00037	50
SPE	LC-DAD	-	0.1	0.005-0.034	this work

Analyte	Sample
Analyte	1	2	3
MPB
Added concentration / (µg mL^-1)	0.50	0.50	0.50
Measured concentration / (µg mL^-1)	0.40	0.44	0.53
RSD / %	20.4	36.2	30.1
Recovery / %	80.7	88.0	105.6
EPB
Added concentration / (µg mL^-1)	0.50	0.50	0.50
Measured concentration / (µg mL^-1)	0.48	0.50	0.54
RSD / %	14.2	15.0	6.6
Recovery / %	97.1	100.2	107.2
PPB
Added concentration / (µg mL^-1)	0.50	0.50	0.50
Measured concentration / (µg mL^-1)	0.51	0.56	0.51
RSD / %	10.8	13.6	10.0
Recovery / %	102.0	112.9	102.0
BPB
Added concentration / (µg mL^-1)	0.50	0.50	0.50
Measured concentration / (µg mL^-1)	0.52	0.59	0.55
RSD / %	10.8	14.6	18.2
Recovery / %	105.2	117.9	110.5

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