Development and Validation of a Rapid and Reliable HPLC-FLD Method for the Quantification of Ciprofloxacin and Enrofloxacin Residues in <i>Zea mays</i>

Brito, Júlio C. M.; Bernardoni, Vinícius; Silva, Thais M. L. da; Ramos, Laurenice S. X. S.; Gomes, Marcelo P.; Assis, Débora C. S. de

doi:10.21577/0103-5053.20210129

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Article • J. Braz. Chem. Soc. 33 (2) • 2022 • https://doi.org/10.21577/0103-5053.20210129 linkcopy

Development and Validation of a Rapid and Reliable HPLC-FLD Method for the Quantification of Ciprofloxacin and Enrofloxacin Residues in Zea mays

Authorship SCIMAGO INSTITUTIONS RANKINGS

Abstract

The accumulation of antibiotics by plants is a currently concern associated to yield reduction and transference of antibiotic residues along the food web. Maize is a staple food in many parts of the world; it is also considered an important ingredient in animal nutrition. Considering the lack of validated analytical methods for the analysis of ciprofloxacin (CIPRO) and enrofloxacin (ENRO) in the shoot of Zea mays maize, we developed a reliable reversed-phase high-performance liquid chromatography method with fluorescence detection (HPLC-FLD). This method was validated for linearity, matrix effects, precision, accuracy, limits of quantification (LOQ) and detection (LOD), and robustness. The analytical curves were linear with coefficient of determination (R²) of 0.9907 for CIPRO and 0.9962 for ENRO. The LOD values were 16.65 and 6.57 μg kg⁻¹ for CIPRO and ENRO, respectively, whereas LOQ values were 50.44 μg kg⁻¹ (CIPRO) and 19.92 μg kg⁻¹ (ENRO). HPLC-FLD also displayed good precision and accuracy. Therefore, the proposed method can be considered a reliable and useful tool for the analysis of ciprofloxacin and enrofloxacin in the shoot of maize.

Keywords:
maize; residue; ciprofloxacin; enrofloxacin; HPLC-FLD; validation

time / min	Mobile phase A / %	Mobile phase B / %	Mobile phase C / %
0	80	12	8
5	80	12	8
8	78	13	9
12	76	14	10
18	5	95	0
21	5	95	0
25	80	12	8

Factor	1	2	3	4	5	6	7	8
A or a	A	A	A	A	a	a	a	a
B or b	B	b	B	b	B	b	B	b
C or c	C	C	c	c	C	C	c	c

Analyte	Equation	R²	r
CIPRO	ENRO	$y = 0.0104 x - 0.0264$	$y = 0.0755 x - 0.4064$
0.9907	0.9962	0.9953	0.9980

Analyte	REC / %			RSD repeat / %			RSD repro / %
Analyte	30 µg kg⁻¹	60 µg kg⁻¹	100 µg kg⁻¹	30 µg kg⁻¹	60 µg kg⁻¹	100 µg kg⁻¹	30 µg kg⁻¹	60 µg kg⁻¹	100 µg kg⁻¹
CIPRO	90.78	105.05	86.49	5.24	11.83	6.46	11.73	9.04	4.32
ENRO	123.1	110.24	108.28	3.75	3.73	4.64	9.35	8.06	3.82

Analyte	LOD / (µg kg⁻¹)	LOQ / (µg kg⁻¹)
CIPRO	16.65	50.44
ENRO	6.57	19.92

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[TFN1] A: phosphate buffer solution 0.5 mol L⁻¹; a: phosphate buffer solution 0.2 mol L⁻¹; B: column temperature 35 ºC; b: column temperature 28 ºC; C: vortex shaking time 2.5 min; c: vortex shaking time 1 min.