Simultaneous determination of pentachlorophenol, niclosamide and fenpropathrin in fishpond water using an LC-MS/MS method for forensic investigation

Jiang, Haipeng; Zhang, Yinhua; Chen, Xiangguo; Lv, Jizhong; Zou, Jing

doi:10.1039/c2ay25685a

Cited by 21 publications

(22 citation statements)

References 20 publications

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“…The deprotonated precursor ions of niclosamide and ibuprofen ([M-H] - ) were detected at m/z of 324.8 and 205.0, respectively, using the negative ionization mode of the ESI interface in the Q1 scan spectra. The transitions of the product ions of niclosamide were observed at m/z 324.8 → 170.9 and 324.8 → 288.8 with negligible difference in sensitivity; however, the m/z 324.8 → 170.9 transition was selected because it presented better linearity, which was similar to that previously reported [15] , [16] . Niclosamide molecules contain two Cl atoms, with a 35 Cl-to- 37 Cl ratio of 3:1.…”

Section: Resultssupporting

confidence: 63%

“…However, information on analytical methods used for niclosamide detection in biological samples and pharmacokinetic analysis in animals is limited. Doran and Stevens [15] and Jiang et al [16] used liquid chromatography–tandem mass spectrometry (LC–MS/MS) for niclosamide detection in water; however, the proposed methods could not be extrapolated to the analysis of biological matrices in general or plasma samples in particular. Chang et al [17] studied the pharmacokinetics of niclosamide in rats; however, the sensitivity, precision, accuracy, and matrix effect of their method for biological samples has not been validated.…”

Section: Introductionmentioning

confidence: 99%

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Bioanalysis of niclosamide in plasma using liquid chromatography-tandem mass and application to pharmacokinetics in rats and dogs

Choi

Kim

Lee

et al. 2021

Journal of Chromatography B

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Niclosamide, which is an anti-tapeworm drug, was developed in 1958. However, recent studies have demonstrated the antiviral effects of niclosamide against the SARS-CoV-2 virus, which causes COVID-19. In this study, we developed and validated a quantitative analysis method for the determination of niclosamide in rat and dog plasma using liquid chromatography–tandem mass spectrometry (LC–MS/MS), and used this method for pharmacokinetic studies. Biological samples were prepared using the protein precipitation method with acetonitrile. Ibuprofen was used as an internal standard. The mobile phase used to quantify niclosamide in rat or dog plasma consisted of 10 mM ammonium formate in distilled water-acetonitrile (30:70, v/v) or 5 mM ammonium acetate-methanol (30:70, v/v). An XDB-phenyl column (5 µm, 2.1 × 50 mm) and a Kinetex® C18 column (5 µm, 2.1 × 500 mm) were used as reverse-phase liquid chromatography columns for rat and dog plasma analyses, respectively. Niclosamide and ibuprofen were detected under multiple reaction monitoring conditions using the electrospray ionization interface running in the negative ionization mode. Niclosamide presented linearity in the concentration ranges of 1-3000 ng/mL (r =0.9967) and 1-1000 ng/mL (r =0.9941) in rat and dog plasma, respectively. The intra- and inter-day precision values were <7.40% and <6.35%, respectively, for rat plasma, and <3.95% and <4.01%, respectively, for dog plasma. The intra- and inter-day accuracy values were <4.59% and <6.63%, respectively, for rat plasma, and <12.1% and <10.9%, respectively, for dog plasma. In addition, the recoveries of niclosamide ranged between 87.8-99.6% and 102-104% for rat and dog plasma, respectively. Niclosamide was stable during storage under various conditions (three freeze-thaw cycles, 6 h at room temperature, long-term, and processed samples). A reliable LC–MS/MS method for niclosamide detection was successfully used to perform pharmacokinetic studies in rats and dogs. Niclosamide presented dose-independent pharmacokinetics in the dose range of 0.3-3 mg/kg after intravenous administration, and drug exposure in rats and dogs after oral administration was very low. Additionally, niclosamide presented high plasma protein binding (>99.8%) and low metabolic stability. These results can be helpful for further developing and understanding the pharmacokinetic characteristics of niclosamide to expand its clinical use.

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Section: Resultssupporting

confidence: 63%

Section: Introductionmentioning

confidence: 99%

Bioanalysis of niclosamide in plasma using liquid chromatography-tandem mass and application to pharmacokinetics in rats and dogs

Choi

Kim

Lee

et al. 2021

Journal of Chromatography B

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“…While LC/MS MS methods for the detection of niclosamide have been developed; many are specific to matrices not representative for in vivo samples (e.g. water or cell culture media), or lack the dynamic range required for application to pharmacokinetic (PK) studies [10][11][12]. The potential application of niclosamide to SARS-CoV-2 therapy presents a bioanalytical challenge because of the paucity of data available publicly for the pharmacokinetics following administration to humans [13].…”

Section: Introductionmentioning

confidence: 99%

Optimisation and validation of a sensitive bioanalytical method for niclosamide

Arshad

Pertinez

Box

et al. 2021

Preprint

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The SARS-CoV-2 pandemic has spread at an unprecedented rate, and repurposing opportunities have been intensively studied with only limited success to date. If successful, repurposing will allow interventions to become more rapidly available than development of new chemical entities. Niclosamide has been proposed as a candidate for repurposing for SARS-CoV-2 based upon the observation that it is amongst the most potent antiviral molecules evaluated in vitro. To investigate the pharmacokinetics of niclosamide, reliable, reproducible and sensitive bioanalytical assays are required. Here, a liquid chromatography tandem mass spectrometry assay is presented which was linear from 31.25-2000 ng/mL (high dynamic range) and 0.78-100 ng/mL (low dynamic range). Accuracy and precision ranged between 97.2% and 112.5%, 100.4% and 110.0%, respectively. The presented assay should have utility in preclinical evaluation of the exposure-response relationship and may be adapted for later evaluation of niclosamide in clinical trials.

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“…Many analytical methods have been used to detect PCP, including electrochemical sensors (Feng et al, 2015), gas chromatography (GC), high-performance liquid chromatography (HPLC) (Yu et al, 2015), liquid chromatography-tandem mass spectrometry (LC-MS/MS) (Jiang, Zhang, Chen, Lv, & Zou, 2013), and gas chromatography-mass spectrometry (GC-MS) (Han, Fang, & Yan, 2005;Kawaguchi et al, 2005;Shen et al, 2014), which are all complex, time-consuming, and expensive. Compared with these methods, an immunoassay is a sensitive, low-cost, and rapid technique that has already been reported to detect PCP (Abuknesha & Griffith, 2004;Emon & Gerlach, 1992;Oubina, Puig, Gascón, & Barceló, 1997;Lee, Ahn, Park, Kang, & Hammock, 2001;Noguera et al, 2002;Xu et al, 2007).…”

Section: Introductionmentioning

confidence: 99%

Development of a highly sensitive ELISA and immunochromatographic strip to detect pentachlorophenol

Sun

Liu

Song

et al. 2016

Food and Agricultural Immunology

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A sensitive monoclonal antibody for targeting pentachlorophenol was prepared with an immunization procedure and cell fusion. The antibody was characterized with an indirect competitive enzymelinked immunosorbent assay (ELISA), which had an IC50 of 0.2 ng/ ml for pentachlorophenol under optimized conditions. The crossreactivity of the ELISA to related compounds was very low. The recovery of pentachlorophenol was 99.2-105% in water samples and 89-110.9% in fish samples. A simple, rapid, and sensitive immunochromatographic strip was produced based on the monoclonal antibody, with a qualitative visual limit of detection of 2 ng/ml in water samples and 10 ng/ml in fish samples, indicating its potential utility in monitoring pentachlorophenol in the field.

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Simultaneous determination of pentachlorophenol, niclosamide and fenpropathrin in fishpond water using an LC-MS/MS method for forensic investigation

Cited by 21 publications

References 20 publications

Bioanalysis of niclosamide in plasma using liquid chromatography-tandem mass and application to pharmacokinetics in rats and dogs

Bioanalysis of niclosamide in plasma using liquid chromatography-tandem mass and application to pharmacokinetics in rats and dogs

Optimisation and validation of a sensitive bioanalytical method for niclosamide

Development of a highly sensitive ELISA and immunochromatographic strip to detect pentachlorophenol

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