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Determination of antibiotic residues in surface water by solid-phase extraction and high-performance liquid chromatography with UV/Vis detection

Epi, Shazalatun Binte Huda LU (2021) KEMR30 20211
Department of Chemistry
Abstract
This work aimed to optimize a multiclass reverse-phase HPLC-DAD chromatographic method and SPE method for the quantification of eight antibiotics in wastewater. Cefalexin, Levofloxacin, Nitrofurantoin, Doxycycline, Nalidixic Acid, Oxacillin sodium salt, and Cloxacillin sodium salt were separated with a C6-Phenyl (100 x 2 mm, 3.00 μm particle size) column within 10 minutes. Gradient elution was performed using mobile phase A: acetonitrile, H2O + ammonium acetate (2mM), formic acid (3/97/0.05, v/v/v) and B Acetonitrile, H2O + ammonium acetate (2mM), formic acid (95/5/0.05, v/v/v). The flow rate was 3.00 mLmin−1, and the injection volume was 3μL. Detection was carried out at wavelength 230 nm using a photodiode array detector. The LOQs ranged... (More)
This work aimed to optimize a multiclass reverse-phase HPLC-DAD chromatographic method and SPE method for the quantification of eight antibiotics in wastewater. Cefalexin, Levofloxacin, Nitrofurantoin, Doxycycline, Nalidixic Acid, Oxacillin sodium salt, and Cloxacillin sodium salt were separated with a C6-Phenyl (100 x 2 mm, 3.00 μm particle size) column within 10 minutes. Gradient elution was performed using mobile phase A: acetonitrile, H2O + ammonium acetate (2mM), formic acid (3/97/0.05, v/v/v) and B Acetonitrile, H2O + ammonium acetate (2mM), formic acid (95/5/0.05, v/v/v). The flow rate was 3.00 mLmin−1, and the injection volume was 3μL. Detection was carried out at wavelength 230 nm using a photodiode array detector. The LOQs ranged from 0.8 to 3.7 μg/mL except for doxycycline and cloxacillin which were 5.3 and 8.1 μg/mL respectively. SPE cartridges and sample pH values were tested both for cleaning and pre-concentrating purposes. It was found that Waters Oasis HLB SPE cartridges were most effective in recovering target compounds from water samples. Furthermore, acidifying samples prior to SPE did not enhance the recovery of the compounds (except Doxycycline and T-HCl). The recovery range was 12% (Cloxacillin) to 166 % (T-HCl). The developed method was not applied to the real sample. (Less)
Popular Abstract
In the modern world, antibiotic resistance is a serious concern. That is why it is essential to identify and quantify antibiotics in different environmental recipients, for example, water sources. Nonetheless, analyzing environmental water samples is not an easy task as it involves complex mixtures of plastics, pathogens, nutrients, chemicals such as antibiotics, pesticides, heavy metals, etc. Sometimes they can also exist at low concentrations. Thus, sample pre-treatment, such as sampling, storage, and cleaning of samples, is essential before antibiotic analysis. Solid-phase extraction is one of the most used sample preparation procedures for extracting samples from water. In this extraction technique, a solid packing material is used for... (More)
In the modern world, antibiotic resistance is a serious concern. That is why it is essential to identify and quantify antibiotics in different environmental recipients, for example, water sources. Nonetheless, analyzing environmental water samples is not an easy task as it involves complex mixtures of plastics, pathogens, nutrients, chemicals such as antibiotics, pesticides, heavy metals, etc. Sometimes they can also exist at low concentrations. Thus, sample pre-treatment, such as sampling, storage, and cleaning of samples, is essential before antibiotic analysis. Solid-phase extraction is one of the most used sample preparation procedures for extracting samples from water. In this extraction technique, a solid packing material is used for cleaning samples. Many commercial solid packing materials are selected based on the chemical properties of the compound. In the next step, the sample needs to be analyzed appropriately. A chromatographic analysis method is one of those methods that is used for separating or analyzing chemical mixtures. The reverse-phase liquid chromatography (RP-HPLC) is one of the chromatography techniques used for separating compounds that are hydrophobic or have less polarity. Since antibiotics are hydrophobic or less polar, RP-HPLC was chosen to analyze them. Mobile and stationary phases are essential components of chromatography.
A stationary phase does not move, whereas a mobile phase is one that moves. When compounds move through the stationary phase, they interact with the stationary phase. Compounds that have a lower attraction with stationary phase will elute first, and the higher attraction will elute later, which are detected by the detector. In RP-HPLC, a partitioning mechanism causes separation through an adsorptive process. Solute molecules are partitioned (i.e. equilibrium is established) between the mobile and stationary phases. When many compounds are mixed, it is difficult to separate them properly. Many terms come into play to separate those compounds properly, e.g., solvent type of flowing them through the stationary phase, pH of the solvent, temperature, etc. Successful separation requires the optimization of all terms together. (Less)
Please use this url to cite or link to this publication:
author
Epi, Shazalatun Binte Huda LU
supervisor
organization
course
KEMR30 20211
year
type
H2 - Master's Degree (Two Years)
subject
keywords
Antibiotics, C6-phenyl column, Gradient elution, Recovery, Solid-phase extraction: Analytical chemistry
language
English
id
9065780
date added to LUP
2021-09-22 15:59:29
date last changed
2021-10-01 10:12:02
@misc{9065780,
  abstract     = {{This work aimed to optimize a multiclass reverse-phase HPLC-DAD chromatographic method and SPE method for the quantification of eight antibiotics in wastewater. Cefalexin, Levofloxacin, Nitrofurantoin, Doxycycline, Nalidixic Acid, Oxacillin sodium salt, and Cloxacillin sodium salt were separated with a C6-Phenyl (100 x 2 mm, 3.00 μm particle size) column within 10 minutes. Gradient elution was performed using mobile phase A: acetonitrile, H2O + ammonium acetate (2mM), formic acid (3/97/0.05, v/v/v) and B Acetonitrile, H2O + ammonium acetate (2mM), formic acid (95/5/0.05, v/v/v). The flow rate was 3.00 mLmin−1, and the injection volume was 3μL. Detection was carried out at wavelength 230 nm using a photodiode array detector. The LOQs ranged from 0.8 to 3.7 μg/mL except for doxycycline and cloxacillin which were 5.3 and 8.1 μg/mL respectively. SPE cartridges and sample pH values were tested both for cleaning and pre-concentrating purposes. It was found that Waters Oasis HLB SPE cartridges were most effective in recovering target compounds from water samples. Furthermore, acidifying samples prior to SPE did not enhance the recovery of the compounds (except Doxycycline and T-HCl). The recovery range was 12% (Cloxacillin) to 166 % (T-HCl). The developed method was not applied to the real sample.}},
  author       = {{Epi, Shazalatun Binte Huda}},
  language     = {{eng}},
  note         = {{Student Paper}},
  title        = {{Determination of antibiotic residues in surface water by solid-phase extraction and high-performance liquid chromatography with UV/Vis detection}},
  year         = {{2021}},
}