Development of a single-step precipitation cleanup method for the determination of enrofloxacin, ciprofloxacin, and danofloxacin in porcine plasma

Choi, Jeong‐Heui; Mamun, M. I. R.; El‐Aty, A. M. Abd; Park, Jong-Hyouk; Shin, Eun-Ho; Park, Ji Yeon; Cho, Soon‐Kil; Shin, Sung Chul; Lee, Kang Bong

doi:10.1016/j.foodchem.2011.02.027

Cited by 27 publications

(10 citation statements)

References 22 publications

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“…However, the recovery of IND from egg was as low as 63% when 1% acetic acid in acetonitrile was used but was between 86 and 106% when the acetic acid content was 0.1%. Acetonitrile containing acid or other additives is typically used as an extraction solvent to precipitate and remove protein (Choi et al, ). However, deproteinization may be hampered by the presence of phospholipids and fatty acids.…”

Section: Resultsmentioning

confidence: 99%

Residue analysis of tebufenozide and indoxacarb in chicken muscle, milk, egg and aquatic animal products using liquid chromatography–tandem mass spectrometry

Choi

Zheng

El‐Aty

et al. 2019

Biomedical Chromatography

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We developed an analytical method using liquid–liquid extraction (LLE) and liquid chromatography–tandem mass spectrometry (LC‐MS/MS) to detect and quantify tebufenozide (TEB) and indoxacarb (IND) residues in animal and aquatic products (chicken muscle, milk, egg, eel, flatfish, and shrimp). The target compounds were extracted using 1% acetic acid (0.1% acetic acid for egg only) in acetonitrile and purified using n‐hexane. The analytes were separated on a Gemini‐NX C18 column using (a) distilled water with 0.1% formic acid and 5 mm ammonium acetate and (b) methanol with 0.1% formic acid as the mobile phase. All six‐point matrix‐matched calibration curves showed good linearity with coefficients of determination (R2) ≥0.9864 over a concentration range of 5–50 μg/kg. Intra‐ and inter‐day accuracy was expressed as the recovery rate at three spiking levels and ranged between 73.22 and 114.93% in all matrices, with a relative standard deviation (RSD, corresponding to precision) ≤13.87%. The limits of quantification (LOQ) of all target analytes ranged from 2 to 20 μg/kg, which were substantially lower than the maximum residue limits (MRLs) specified by the regulatory agencies of different countries. All samples were collected from different markets in Seoul, Republic of Korea, and tested negative for tebufenozide and indoxacarb residues. These results show that the method developed is robust and may be a promising tool to detect trace levels of the target analytes in animal products.

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Section: Resultsmentioning

confidence: 99%

Residue analysis of tebufenozide and indoxacarb in chicken muscle, milk, egg and aquatic animal products using liquid chromatography–tandem mass spectrometry

Choi

Zheng

El‐Aty

et al. 2019

Biomedical Chromatography

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“…The PS-USLM method developed and optimized in this study was compared with other previously reported methods, such as liquid-liquid extraction combined with HPLC (LLE-HPLC) [27], solid-phase extraction combined with HPLC (SPE-HPLC) [29], second-order multivariate calibration combined with HPLC (SOMC-HPLC) [30], single-step precipitation cleanup method combined with HPLC (SSPC-HPLC) [31], direct ultra-fast liquid chromatography (UFLC) [32], and hollow fiber-based liquid phase microextraction combined with HPLC (HF-LPME-HPLC) [33]. The results were compared with reference to sample preparation time, LOD, RR, extraction solvent and injection method.…”

Section: Comparison Of Ps-uslm With Other Pretreatment Methodsmentioning

confidence: 99%

Integration of phase separation with ultrasound-assisted salt-induced liquid–liquid microextraction for analyzing the fluoroquinones in human body fluids by liquid chromatography

Wang

Gao

Wang

et al. 2015

Journal of Chromatography B

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a b s t r a c tHerein, we developed a novel integrated device to perform phase separation based on ultrasound-assisted salt-induced liquid-liquid microextraction for determination of five fluoroquinones (FQs) in human body fluids. The integrated device consisted of three simple HDPE components used to separate the extraction solvent from the aqueous phase prior to retrieving the extractant. A series of extraction parameters were optimized using the response surface method based on central composite design. Optimal conditions consisted of 945 L acetone extraction solvent, pH 2.1, 4.1 min stir time, 5.9 g Na 2 SO 4 , and 4.0 min centrifugation. Under optimized conditions, the limits of detection (at S/N = 3) were 0.12-0.66 g L −1 , the linear range was 0.5-500 g L −1 and recoveries were 92.6-110.9% for the five FQs extracted from plasma and urine. The proposed method has several advantages, such as easy construction from inexpensive materials, high extraction efficiency, short extraction time, and compatibility with HPLC analysis. Thus, this method shows excellent prospects for sample pretreatment and analysis of FQs in human body fluids.© 2015 Elsevier B.V. All rights reserved.Abbreviations: PS-USLM, phase separation based on ultrasound-assisted, salt-induced, liquid-liquid microextraction; FQs, fluoroquinones; HPLC-FLD, high performance liquid chromatography equipped with fluorescence detector; PPCPs, pharmaceuticals and personal care products; HPLC, high performance liquid chromatography; MS, mass spectrometry; SPE, solid-phase extraction; LLE, liquid-liquid extraction; LPME, liquid-phase microextraction; DLLME, dispersive liquid-liquid microextraction; SALLME, salting-out assisted liquid-liquid microextraction; RSM, response surface method; CCD, central composite design; LOD, limits of detection; ER, extraction recovery; FLE, fleroxacin; OFL, ofloxacin; NOR, norfloxacin; CIP, ciprofloxacin; ENR, enrofloxacin; MgSO4, magnesium sulfate; Na2SO4, sodium sulfate; CH3COONa, sodium acetate; (NH4)2SO4, ammonium sulfate; CH3COONH4, ammonium acetate; HDPE, high-density polyethylene; LDR, linear dynamic range; RSDs, relative standard deviations; RR, relative recovery; LLE-HPLC, liquid-liquid extraction combined with high performance liquid chromatography; SPE-HPLC, solid phase extraction combined with high performance liquid chromatography; SOMC-HPLC, second-order multivariate calibration combined with high performance liquid chromatography; SSPC-HPLC, single-step precipitation cleanup method combined with high performance liquid chromatography; UFLC, ultra-fast liquid chromatography; HF-LPME-HPLC, hollow fiber-based liquid phase microextraction combined with high performance liquid chromatography.

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“…Various analytical techniques have been employed for the determination of CIP. Among the most often used techniques belongs the high‐performance liquid chromatography (HPLC) with fluorescence , ultraviolet and particularly with mass spectrometric detection.…”

Section: Introductionmentioning

confidence: 99%

Heavily Boron Doped Diamond Electrodes for Ultra Sensitive Determination of Ciprofloxacin in Human Urine

et al. 2017

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Ciprofloxacin is one of the most potent fluoroquinolone antibiotics in medical treatment with a widely effective antibacterial activity. Aim of the presented paper was to use boron doped diamond electrodes for a sensitive, simple and reliable voltammetric determination of ciprofloxacin in human urine samples. Prior to the electrochemical analyses, an optimal boron doping level was determined in order to achieve the highest sensitivity. A set of boron doped diamond electrodes with the doping level in the range from 0 to 20 000 ppm B/C was used for this purpose. Electrochemical behavior of ciprofloxacin was investigated using cyclic voltammetry in an ammonium acetate buffer (pH 5), where ciprofloxacin provided a well‐defined irreversible oxidation peak at a potential of + 1.15 V. Under optimal experimental conditions, the calibration curve obtained by square‐wave voltammetry was linear in a concentration range from 0.15 to 2.11 μmol/L (R2=0.9974). A very low limit of detection (0.05 μmol/L) was obtained for the BDD electrode with the highest doping level. The developed square wave method was successfully applied to the determination of ciprofloxacin in human urine samples with a very good recovery (from 97 to 102%).

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Development of a single-step precipitation cleanup method for the determination of enrofloxacin, ciprofloxacin, and danofloxacin in porcine plasma

Cited by 27 publications

References 22 publications

Residue analysis of tebufenozide and indoxacarb in chicken muscle, milk, egg and aquatic animal products using liquid chromatography–tandem mass spectrometry

Residue analysis of tebufenozide and indoxacarb in chicken muscle, milk, egg and aquatic animal products using liquid chromatography–tandem mass spectrometry

Integration of phase separation with ultrasound-assisted salt-induced liquid–liquid microextraction for analyzing the fluoroquinones in human body fluids by liquid chromatography

Heavily Boron Doped Diamond Electrodes for Ultra Sensitive Determination of Ciprofloxacin in Human Urine

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