Facile preparation of magnetic graphene oxide/nanoscale zerovalent iron adsorbent for magnetic solid‐phase extraction of ultra‐trace quinolones in milk samples

Wei, Dan; Guo, Mengping

doi:10.1002/jssc.202000108

Cited by 21 publications

(5 citation statements)

References 22 publications

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“…However, during this time, at least 10 samples can be prepared simultaneously (this number corresponds to the number of places on the shaker). The overall analysis time of our methodology is similar to that of the MSPE-HPLC–MS method 28 (72 min) or SDME-CE procedure 5 (61 min), but much shorter than in EEM-ANWE approach 10 (155 min).…”

Section: Resultsmentioning

confidence: 74%

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Simple, fast and reliable CE method for simultaneous determination of ciprofloxacin and ofloxacin in human urine

Kośka

Purgat

Kubalczyk

2022

Sci Rep

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A simple, fast, and accurate capillary zone electrophoresis method has been developed for the determination of ciprofloxacin and ofloxacin. This method uses liquid–liquid extraction. Therefore, it is characterized by a very simple procedure of sample preparation but at the same time satisfactory precision and accuracy. The extraction process of the same urine sample was repeated three times. The extraction protocol was performed each time for 15 min with 1 mL of dichloromethane and chloroform mixture in a 3:1 volume ratio. A 0.1 mol/L phosphate-borate buffer (pH 8.40) was selected as the background electrolyte. UV detection was performed at 288 nm. The separation was carried out at a voltage of 16 kV, at a temperature of 25 °C. Experimentally evaluated LOQ values for ciprofloxacin and ofloxacin were 0.2 nmol/mL urine and 0.05 nmol/mL urine, respectively. For both analytes the calibration curves exhibited linearity over the entire tested concentration range of 1–6 nmol/mL urine. The precision of the method did not exceed 15%, and the recovery was in the range of 85–115%. The developed and validated procedure was applied to analyze human urine for the content of ciprofloxacin and ofloxacin.

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Section: Resultsmentioning

confidence: 74%

“…The LOD and LOQ values evaluated for Cpx were: 0.05 and 0.2 nmol/mL urine and for Ofx were 0.01 nmol/mL urine and 0.05 nmol/mL urine, respectively. The LOD and LOQ of the developed method are lower than for CE procedure 26 and CIEF method 27 but higher than for UPLC-MS/MS method 1 and MSPE-HPLC–MS procedure 28 (Table 2 ).…”

Section: Resultsmentioning

confidence: 93%

Simple, fast and reliable CE method for simultaneous determination of ciprofloxacin and ofloxacin in human urine

Kośka

Purgat

Kubalczyk

2022

Sci Rep

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“…In this method, the LOD and LOQ values for both analytes were 0.04 nmol/g tissue and 0.15 nmol/g tissue (5 ng/mL for Cpx and 5.4 ng/mL for Ofx), respectively. The LOD and LOQ values for our procedure were higher than for the methods that use MS detection [ 1 ]: the LOD value for Cpx and Ofx was 0.005 ng/mL and the LOQ value was 0.015 ng/mL for both analytes [ 32 ]; the LOD values for Cpx and Ofx were 0.15 ng/L and 3.0 ng/L, respectively; the LOQ for Cpx and Ofx was 0.2 ng/L and 10 ng/L, respectively [ 33 ]; the LOD value for Cpx and Ofx was 10.1 ng/L and 3.1 ng/L, respectively; the values of LOQ for Cpx and Ofx were 33.8 and 10.4 ng/L, respectively. However, they were lower than for the CIEF method [ 34 ] (LOD value for Cpx was 0.34 µg/mL and for Ofx was 1.20 µg/mL) and for other CE procedures [ 35 ] (for Cpx, the LOQ value was 0.0125 mg/mL).…”

Section: Resultsmentioning

confidence: 99%

The Use of Extraction on C18-Silica-Modified Magnetic Nanoparticles for the Determination of Ciprofloxacin and Ofloxacin in Meat Tissues

Kośka,

Kubalczyk,

Cichomski

et al. 2023

Molecules

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A simple, fast, and low-cost method of extraction using magnetic nanoparticles was developed for sample preparation in the determination of ciprofloxacin and ofloxacin in meat tissues with the use of capillary electrophoresis. This study is the first utilization of silica-coated magnetic nanoparticles with attached C18 chains to extract fluoroquinolones from meat tissues. This method is therefore characterized by a very simple sample preparation procedure, but on the other hand, by satisfactory precision and accuracy. Magnetic nanoparticles with an appropriately modified surface were placed in an Eppendorf tube, then conditioned with methanol, next rinsed with water and, finally, a homogenized tissue sample was added. At the neutral pH of the sample solution, these compounds do not have a charge and are able to adsorb on the modified particles. After extraction, the nanoparticles were dried and, then, desorption of analytes was conducted with the use of a mixture of 0.1 mol/L HCl and acetonitrile (1:1). This approach made it possible to purify the sample matrix and to obtain satisfactory LOQ levels for the method using the CE technique with UV-Vis detection. In this method, the LOD and LOQ values for both analytes were 0.04 nmol/g tissue and 0.15 nmol/g tissue, respectively. The calibration curves were linear in the entire concentration range, and the accuracy and the recovery of the method were at the satisfactory levels. The square value of the linear correlation coefficients (R2) for Cpx and Ofx were 0.9995 and 0.9992, respectively. The precision value of the method was within the range of 3–11% and accuracy was in the range of 93–110%.

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“…The overall time needed to prepare and analyze the meat sample for Cpx and Ofx content equals 55 min (during this time, seven samples can be prepared simultaneously due to the seven places in the vortex). This analysis time is shorter in the magnetic solid-phase extraction HPLC-MS [24] (72 min), single drop microextraction CE [12] (61 min), and excitation-emission matrix with an alternating normalization-weighted error (EEM-ANWE) [25] (155 min) procedure.…”

Section: Calibration and Other Validation Datamentioning

confidence: 99%

Simultaneous Determination of Ciprofloxacin and Ofloxacin in Animal Tissues with the Use of Capillary Electrophoresis with Transient Pseudo-Isotachophoresis

et al. 2021

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We have developed a precise and accurate method for the determination of ciprofloxacin and ofloxacin in meat tissues. Our method utilizes capillary electrophoresis with a transient pseudo-isotachophoresis mechanism and liquid–liquid extraction during sample preparation. For our experiment, a meat tissue sample was homogenized in pH 7.00 phosphate buffer at a ratio of 1:10 (tissue mass: buffer volume; g/mL). The extraction of each sample was carried out twice for 15 min with 600 µL of a mixture of dichloromethane and acetonitrile at a 2:1 volume ratio. We then conducted the electrophoretic separation at a voltage of 16 kV and a temperature of 25 °C using a background electrolyte of 0.1 mol/L phosphate–borate (pH 8.40). We used the UV detection at 288 nm. The experimentally determined LOQs for ciprofloxacin and ofloxacin were 0.27 ppm (0.8 nmol/g tissue) and 0.11 ppm (0.3 nmol/g tissue), respectively. The calibration curves exhibited linearity over the tested concentration range of 2 to 10 nmol/g tissue for both analytes. The relative standard deviation of the determination did not exceed 15%, and the recovery was in the range of 85–115%. We used the method to analyze various meat tissues for their ciprofloxacin and ofloxacin contents.

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Facile preparation of magnetic graphene oxide/nanoscale zerovalent iron adsorbent for magnetic solid‐phase extraction of ultra‐trace quinolones in milk samples

Cited by 21 publications

References 22 publications

Simple, fast and reliable CE method for simultaneous determination of ciprofloxacin and ofloxacin in human urine

Simple, fast and reliable CE method for simultaneous determination of ciprofloxacin and ofloxacin in human urine

The Use of Extraction on C18-Silica-Modified Magnetic Nanoparticles for the Determination of Ciprofloxacin and Ofloxacin in Meat Tissues

Simultaneous Determination of Ciprofloxacin and Ofloxacin in Animal Tissues with the Use of Capillary Electrophoresis with Transient Pseudo-Isotachophoresis

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