Response Surface Optimization of a Rapid Ultrasound-Assisted Extraction Method for Simultaneous Determination of Tetracycline Antibiotics in Manure

A rapid and cleanup-free ultrasound-assisted extraction method is proposed for the simultaneous extraction of oxytetracycline, tetracycline, chlortetracycline, and doxycycline in manure. The analytes were determined using high-performance liquid chromatography with ultraviolet detector. The influenc...

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Main Authors: Lanqing Li, Mingxing Sun, Hui Zhou, Yun Zhou, Ping Chen, Hong Min, Guoqing Shen
Format: Article
Language:English
Published: Wiley 2015-01-01
Series:Journal of Analytical Methods in Chemistry
Online Access:http://dx.doi.org/10.1155/2015/290903
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author Lanqing Li
Mingxing Sun
Hui Zhou
Yun Zhou
Ping Chen
Hong Min
Guoqing Shen
author_facet Lanqing Li
Mingxing Sun
Hui Zhou
Yun Zhou
Ping Chen
Hong Min
Guoqing Shen
author_sort Lanqing Li
collection DOAJ
description A rapid and cleanup-free ultrasound-assisted extraction method is proposed for the simultaneous extraction of oxytetracycline, tetracycline, chlortetracycline, and doxycycline in manure. The analytes were determined using high-performance liquid chromatography with ultraviolet detector. The influence of several variables on the efficiency of the extraction procedure was investigated by single-factor experiments. The temperature, pH, and amount of extraction solution were selected for optimization experiment using response surface methodology. The calibration curves showed good linearity (R2>0.99) for all analytes in the range of 0.1–20 μg/mL. The four antibiotics were successfully extracted from manure with recoveries ranging from 81.89 to 92.42% and good reproducibility (RSD, <4.06%) under optimal conditions, which include 50 mL of McIlvaine buffer extraction solution (pH 7.15) mixed with 1 g of manure sample, extraction temperature of 40°C, extraction time of 10 min, and three extraction cycles. Method quantification limits of 1.75–2.32 mg/kg were obtained for the studied compounds. The proposed procedure demonstrated clear reductions in extraction time and elimination of cleanup steps. Finally, the applicability to tetracyclines antibiotics determination in real samples was evaluated through the successful determination of four target analytes in swine, cow manure, and mixture of animal manure with inorganic fertilizer.
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language English
publishDate 2015-01-01
publisher Wiley
record_format Article
series Journal of Analytical Methods in Chemistry
spelling doaj-art-de1e0ec2d6884c3aa27b54305b5b2b3c2025-02-03T01:01:51ZengWileyJournal of Analytical Methods in Chemistry2090-88652090-88732015-01-01201510.1155/2015/290903290903Response Surface Optimization of a Rapid Ultrasound-Assisted Extraction Method for Simultaneous Determination of Tetracycline Antibiotics in ManureLanqing Li0Mingxing Sun1Hui Zhou2Yun Zhou3Ping Chen4Hong Min5Guoqing Shen6Department of Environment and Resource, School of Agriculture and Biology, Shanghai Jiao Tong University, Shanghai 200240, ChinaShanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, ChinaShanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, ChinaShanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, ChinaDepartment of Environment and Resource, School of Agriculture and Biology, Shanghai Jiao Tong University, Shanghai 200240, ChinaShanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, ChinaDepartment of Environment and Resource, School of Agriculture and Biology, Shanghai Jiao Tong University, Shanghai 200240, ChinaA rapid and cleanup-free ultrasound-assisted extraction method is proposed for the simultaneous extraction of oxytetracycline, tetracycline, chlortetracycline, and doxycycline in manure. The analytes were determined using high-performance liquid chromatography with ultraviolet detector. The influence of several variables on the efficiency of the extraction procedure was investigated by single-factor experiments. The temperature, pH, and amount of extraction solution were selected for optimization experiment using response surface methodology. The calibration curves showed good linearity (R2>0.99) for all analytes in the range of 0.1–20 μg/mL. The four antibiotics were successfully extracted from manure with recoveries ranging from 81.89 to 92.42% and good reproducibility (RSD, <4.06%) under optimal conditions, which include 50 mL of McIlvaine buffer extraction solution (pH 7.15) mixed with 1 g of manure sample, extraction temperature of 40°C, extraction time of 10 min, and three extraction cycles. Method quantification limits of 1.75–2.32 mg/kg were obtained for the studied compounds. The proposed procedure demonstrated clear reductions in extraction time and elimination of cleanup steps. Finally, the applicability to tetracyclines antibiotics determination in real samples was evaluated through the successful determination of four target analytes in swine, cow manure, and mixture of animal manure with inorganic fertilizer.http://dx.doi.org/10.1155/2015/290903
spellingShingle Lanqing Li
Mingxing Sun
Hui Zhou
Yun Zhou
Ping Chen
Hong Min
Guoqing Shen
Response Surface Optimization of a Rapid Ultrasound-Assisted Extraction Method for Simultaneous Determination of Tetracycline Antibiotics in Manure
Journal of Analytical Methods in Chemistry
title Response Surface Optimization of a Rapid Ultrasound-Assisted Extraction Method for Simultaneous Determination of Tetracycline Antibiotics in Manure
title_full Response Surface Optimization of a Rapid Ultrasound-Assisted Extraction Method for Simultaneous Determination of Tetracycline Antibiotics in Manure
title_fullStr Response Surface Optimization of a Rapid Ultrasound-Assisted Extraction Method for Simultaneous Determination of Tetracycline Antibiotics in Manure
title_full_unstemmed Response Surface Optimization of a Rapid Ultrasound-Assisted Extraction Method for Simultaneous Determination of Tetracycline Antibiotics in Manure
title_short Response Surface Optimization of a Rapid Ultrasound-Assisted Extraction Method for Simultaneous Determination of Tetracycline Antibiotics in Manure
title_sort response surface optimization of a rapid ultrasound assisted extraction method for simultaneous determination of tetracycline antibiotics in manure
url http://dx.doi.org/10.1155/2015/290903
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