Aqueous Ultrasound-Assisted Extraction for the Determination of Fluoroquinolones in Mangrove Sediment by High-Performance Liquid Chromatography and Fluorescence Detector

Neves, Mônica A.; Silva, Gilmar S.; Brito, Natilene M.; Araújo, Karla C. M.; Marques, Edmar P.; Silva, Lanna K.

doi:10.21577/0103-5053.20170108

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Articles • J. Braz. Chem. Soc. 29 (1) • Jan 2018 • https://doi.org/10.21577/0103-5053.20170108 copy

Aqueous Ultrasound-Assisted Extraction for the Determination of Fluoroquinolones in Mangrove Sediment by High-Performance Liquid Chromatography and Fluorescence Detector

Authorship SCIMAGO INSTITUTIONS RANKINGS

A method for simultaneous analysis of ciprofloxacin (CIP), levofloxacin (LEV) and norfloxacin (NOR) in mangrove sediment was developed using aqueous ultrasound-assisted extraction (UAE), solid phase extraction (SPE) and high-performance liquid chromatography with fluorescence detection (HPLC-FD). The method showed excellent linear correlation coefficient for the three fluoroquinolones (r² > 0.999) using external calibration curve and good recovery in real sediment samples ranging from 73.73 to 88.85%. The precision showed a relative standard deviation lower than 20% and detection limits of 1.10, 3.33 and 0.26 µg kg^-1 to CIP, LEV and NOR, respectively. There was no presence of interfering. After validation, the method was applied in the determination of pharmaceuticals in mangrove sediment in the Paciência River, Maranhão Island, Brazil. Only the CIP antibiotic was found in three of six samples analyzed, with values ranging 56.55-70.45 µg kg^-1.

Keyword:
fluoroquinolones; sediment; ultrasound assisted extraction; solid phase extraction

Compound	pK_a	log K_ow^a a log Kow and Kd were presented as minimum and maximum/mean; ,^b b depending on reference denoted as Kow, Pow, Papp, or D.	K_d^a a log Kow and Kd were presented as minimum and maximum/mean; (soil) / (L kg^-1)	K_d^a a log Kow and Kd were presented as minimum and maximum/mean; (sediment) / (L kg^-1)	Zwitterionic point (pH)	Reference
CIP	pK_a1 = 5.90 pK_a2 = 8.89	-2.82; 2.30/-0.81	74; 1,277,874/21,099	794; 18,620/7,000	7.5	¹⁴14 Tolls, J.; Environ. Sci. Technol. 2001, 35, 3397. 15 Vasudevan, D.; Bruland, G. L.; Torrance, B. S.; Upchurch, V. G.; MacKay, A.; Geoderma 2009, 151, 68. ^- ¹⁶16 Van Doorslaer, X.; Dewulf, J.; Van Langenhove, H.; Demeestere, K.; Sci. Total Environ. 2014, 500-501, 250.
LEV	pK_a1 = 5.59 pK_a2 = 7.94	-2.00; 1.30/-0.72	-	-	6.77	¹⁶16 Van Doorslaer, X.; Dewulf, J.; Van Langenhove, H.; Demeestere, K.; Sci. Total Environ. 2014, 500-501, 250. 17 Ahmad, I.; Bano, R.; Sheraz, M. A.; Ahmed, S.; Mirza, T.; Ansari, S. A.; Acta Pharm. 2013, 63, 223. ^- ¹⁸18 Sarisaltik, D.; Teksin, Z. F.; FABAD J. Pharm. Sci. 2007, 32, 197.
NOR	pK_a1 = 6.20 pK_a2 = 8.55	-3.78; 1.45/-1.17	41; 335,633/29,876	30; 75/54	7.34	¹⁴14 Tolls, J.; Environ. Sci. Technol. 2001, 35, 3397. ^, ¹⁶16 Van Doorslaer, X.; Dewulf, J.; Van Langenhove, H.; Demeestere, K.; Sci. Total Environ. 2014, 500-501, 250. ^, ¹⁹19 Uivarosi, V.; Molecules 2013, 18, 11153.

Method^a a Volume extraction (10 mL), extraction cycles (3) and extraction time (15 min) are the same for all methods.	Extraction solution	Reference
1	0.2 M phosphate buffer solution (pH 3.0) and methanol 50:50 (v/v)	²⁶26 Yang, J. F.; Ying, G. G.; Zhao, J. L.; Tao, R.; Su, H. C.; Chen, F.; Sci. Total Environ. 2010, 408, 3424.
2	0.2 M citrate buffer solution (pH 4.0) and acetonitrile 50:50 (v/v)	³⁴34 Uslu, M. Ö.; Yediler, A.; Balcıoğlu, I. A.; Schulte-Hostede, S.; Water, Air, Soil Pollut. 2008, 1901, 55.
3	aqueous solution of Mg(NO₃)₂ to 29% (m/v) (pH 8.1) adjusted with ammonia 4% (v/v)	³⁵35 Turiel, E.; Martín-Esteban, A.; Tadeo, J. L.; Anal. Chim. Acta 2006, 562, 30.

Analyte	Retention time / min	Linear equation	r²
LEV	10.4	y = 0.451x + 0.443	0.9997
NOR	12.3	y = 3.163x - 4.771	0.9999
CIP	13.6	y = 2.655x - 2.198	0.9999

Analyte	LOD / (µg kg^-1)	LOQ / (µg kg^-1)
CIP	1.10	3.68
LEV	3.33	11.10
NOR	0.26	0.86

Analyte	Spiked level / (µg kg^-1)	Recovery / %	RSD / %
CIP	20	76.67	8.79
	200	73.73	4.26
	500	76.43	3.60
LEV	20	85.73	2.51
	200	88.85	3.96
	500	87.64	6.57
NOR	20	81.52	4.71
	200	82.85	2.62
	500	85.63	6.49

Site	CIP ± SD / (µg kg^-1)	LEV ± SD / (µg kg^-1)	NOR ± SD / (µg kg^-1)
1	60.08 ± 5.56	n.d	n.d
2	n.d	n.d	n.d
3	70.45 ± 4.81	n.d	n.d
4	n.d	n.d	n.d
5	56.55 ± 4.45	n.d	n.d
6	n.d	n.d	n.d

Region	Fluoroquinolone	Concentration	Reference
Rio Pearl, China	CIP NOR	9.02-197 µg kg^-1 19.2-1120 µg kg^-1	²⁶26 Yang, J. F.; Ying, G. G.; Zhao, J. L.; Tao, R.; Su, H. C.; Chen, F.; Sci. Total Environ. 2010, 408, 3424.
Valência, Spain	CIP	5.95 ng g^-1	²⁸28 Vazquez-Roig, P.; Segarra, R.; Blasco, C.; Andreu, V.; Picó, Y.; J. Chromatogr. A 2010, 1217, 2471.
Yellow, Hai and Liao Rivers, China	CIP NOR	32.8; 1290; 28.7 ng g^-1 141; 5770; 176 ng g^-1	³⁶36 Zhou, L. J.; Ying, G. G.; Zhao, J. L.; Yang, J. F.; Wang, L.; Yang, B.; Liu, S.; Environ. Pollut. 2011, 159, 1877.
Baiyangdian Lake, China	CIP NOR	2.49 µg kg^-1 267 µg kg^-1	⁶⁰60 Wenhui, L.; Yali, S.; Lihong, G.; Jiemin, L.; Yaqi, C.; Chemosphere 2012, 89, 1307.
Paciência River, São Luís-MA, Brazil	CIP	56.6-70.4 µg kg^-1	this study

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