Determination of Bithionol, Bromophen, Nitroxynil, Oxyclozanide, and Tribromsalan in Milk with Liquid Chromatography Coupled with Tandem Mass Spectrometry

Takeba, Kazue; Sasamoto, Takeo; Kusano, Tomoko; Hayashi, Hiroshi; Kanai, Setsuko; Kanda, Manabu; Nagayama, Toshihiro

doi:10.1093/jaoac/93.4.1340

Cited by 15 publications

(9 citation statements)

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“…Full ESI scans were performed in both ESI (±) detection modes to optimize the mass spectrometry parameters for oxyclozanide and the IS. Better MS responses were achieved in ESI (−) mode compared with ESI (+) mode, consistent with previous reports [16, 18, 19]. The choice of the IS is particularly important, as it provides a baseline value for the continuous monitoring of the performance of the chromatograph and mass spectrometer during analysis, and affects the precision and accuracy of the method [29, 30].…”

Section: Discussionsupporting

confidence: 85%

“…Instead, some methods have recently been developed to detect oxyclozanide residues in dairy animals. For example, levels of oxyclozanide residues in milk have been measured using ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) and liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) methods [16–18]. Meanwhile, the stability of oxyclozanide residues in beef during cooking has been analysed using a UPLC-MS/MS method [19].…”

Section: Introductionmentioning

confidence: 99%

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Determination and pharmacokinetics study of oxyclozanide suspension in cattle by LC-MS/MS

Zhang

Bai

et al. 2019

BMC Vet Res

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Background Oxyclozanide is an anthelmintic drug that is widely used to treat fasciolosis . However, the pharmacokinetics of oxyclozanide in cattle are not yet clearly understood. The present study was designed to develop a sensitive method to determine oxyclozanide levels in cattle plasma using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) and to study its pharmacokinetics for application in cattle. Results A simple and rapid HPLC-MS/MS analytical method was established and validated to quantify oxyclozanide levels in cattle plasma using niclosamide as the internal standard (IS) in negative ion mode. Chromatographic separation of the analytes was achieved using a C 18 analytical column (75 × 4.6 mm, 2.7 μm) at 30 °C. The mobile phase comprised 0.01% v/v acetic acid (HOAc) diluted in water:acetonitrile (MeCN) (90:10% v/v) and 5 mM ammonium formate in methanol (MeOH):MeCN (75:25, v/v) at a 10:90 ratio (v/v) and was delivered at a flow rate of 0.4 mL min − 1 . A good linear response across the concentration range of 0.02048–25.600 μg/mL was achieved (r 2 = 0.994). The method was validated with respect to linearity, matrix effect, accuracy, precision, recovery and stability. The lower limit of quantification (LLOQ) was 0.020 μg/mL, and the extraction recovery was > 98% for oxyclozanide. The inter- and intra-day accuracy and precision of the method showed the relative standard deviation (RSD) less than 10%. The method was successfully applied to an assessment of the pharmacokinetics of oxyclozanide in cattle plasma. In healthy cattle, a single oral dose of an oxyclozanide suspension followed the one-compartment model, with a half-life (T 1/2 ) of 64.40 ± 30.18 h, a plasma clearance rate (CL/F) of 11.426 ± 2.442 mL/h/kg, and an average area under the curve (AUC) of 965.608 ± 220.097 h*μg/mL. The peak concentration (C max ) was 15.870 ± 2.855 μg/mL, which occurred at a peak time (T max ) = 22.032 ± 3.343 h. Conclusions A reliable, accurate HPLC-MS/MS analytical method was established in our study and successful applied to study the pharmacokinetics of oxyclozanide in cattle plasma. These results will be useful for further evaluations of the pharmacokinetic properties of oxyclozanide or for monitoring therapeutic drugs in animals.

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Section: Discussionsupporting

confidence: 85%

Section: Introductionmentioning

confidence: 99%

Determination and pharmacokinetics study of oxyclozanide suspension in cattle by LC-MS/MS

Zhang

Bai

et al. 2019

BMC Vet Res

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“…Oxyclozanide is also used to treat infections caused by F. gigantic and F. hepatica [6]. Very few papers, most of them are spectrophotometric and chromatographic analytical methods, have been reported in the literature for the determination of oxyclozanide in veterinary medicinal products and biological fluids such as liquid chromatography [7], high-performance liquid chromatography (HPLC) [8,9], high-performance thin-layer chromatography [10], HPLC-tandem mass spectrometry [11], liquid chromatography coupled with tandem mass spectrometry [12] and spectrophotometry [13]. These methods are widely used in routine analysis since they are good in sensitivity, stability and repeatability.…”

Section: Introductionmentioning

confidence: 99%

Development of a New Analytical Method for Determination of Veterinary Drug Oxyclozanide by Electrochemical Sensor and Its Application to Pharmaceutical Formulation

Demir

Silah

2020

Chemosensors

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A novel highly selective, sensitive and simple analytical technique was recommended for the investigation of anthelmintic veterinary drug oxyclozanide based on square wave anodic stripping voltammetry (SWASV) by using a carbon paste electrode (CPE). According to the cyclic voltammetric data, the oxidation and electron transfer processes of oxyclozanide were found as irreversible and adsorption-controlled, respectively. The voltammetric anodic peak response was characterized with respect to pH, accumulation potential, accumulation time, frequency and pulse amplitude, etc. Under these optimized experimental conditions, the anodic peak density of oxyclozanide was linear to oxyclozanide concentrations in the range from 0.058 to 4.00 mg/L. The described electrochemical method was successfully carried out for the oxyclozanide in pharmaceutical formulation and tap water with mean percentage recovery of 101.5 % and 102.2 %, respectively. The results of pharmaceutical formulation studies were statistically compared to the high-performance liquid chromatographic method.

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“…Many techniques for the detection of NIT in milk have been reported in the literature, such as ultra‐performance liquid chromatography coupled with tandem mass spectrometry (UPLC/MS), liquid chromatography coupled with tandem mass spectrometry (LC/MS), gas chromatography (GC), high‐performance liquid chromatography (HPLC) and so on. These methods have excellent accuracy and sensitivity.…”

Section: Introductionmentioning

confidence: 99%

A rapid colloidal gold‐based immunochromatographic strip assay for monitoring nitroxynil in milk

Yang

et al. 2020

J Sci Food Agric

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BACKGROUND Nitroxynil (NIT) is a veterinary drug against hepatic fluke disease for food‐producing cattle and sheep. NIT has a long half‐life time in animals since it is highly bound to plasma protein. Therefore NIT possibly remains in animal edible tissues or milk due to drug abuse. In this study, a specific murine monoclonal antibody (mAb) against NIT was prepared and an immunochromatographic strip assay based on the mAb was developed for screening NIT in milk. RESULTS The affinity constant of the anti‐NIT mAb was 2.93 × 1010 and the anti‐NIT mAb had almost no cross‐reactivity with other analogs, so that it showed good specificity. The cutoff value of this test strip was considered to be 50 ng mL−1 by the naked eye. When detected by the strip reader, the half maximum inhibition concentration (IC50) of the immunoassay strip was calculated to be 5.716 ng mL−1 and the limit of detection (LOD) was 1.146 ng mL−1. Intra‐assay recoveries from 88.80 to 97.13% were obtained, with the highest coefficient of variation (CV) at 9.01%; inter‐assay recoveries ranged from 84.60 to 106.87%, with the highest CV at 9.93%. CONCLUSION The operative procedure of the proposed method can be completed within 10 min. The strip developed in this study was a practical tool for rapid semiquantitative and quantitative detection of NIT in milk. This study suggested great potential for analytically monitoring NIT in other food samples. © 2019 Society of Chemical Industry

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Determination of Bithionol, Bromophen, Nitroxynil, Oxyclozanide, and Tribromsalan in Milk with Liquid Chromatography Coupled with Tandem Mass Spectrometry

Cited by 15 publications

References 0 publications

Determination and pharmacokinetics study of oxyclozanide suspension in cattle by LC-MS/MS

Determination and pharmacokinetics study of oxyclozanide suspension in cattle by LC-MS/MS

Development of a New Analytical Method for Determination of Veterinary Drug Oxyclozanide by Electrochemical Sensor and Its Application to Pharmaceutical Formulation

A rapid colloidal gold‐based immunochromatographic strip assay for monitoring nitroxynil in milk

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