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      A Liquid Chromatography – Tandem Mass Spectrometry Approach for the Identification of Mebendazole Residue in Pork, Chicken, and Horse

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          Abstract

          A confirmatory and quantitative method of liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the determination of mebendazole and its hydrolyzed and reduced metabolites in pork, chicken, and horse muscles was developed and validated in this study. Anthelmintic compounds were extracted with ethyl acetate after sample mixture was made alkaline followed by liquid chromatographic separation using a reversed phase C 18 column. Gradient elution was performed with a mobile phase consisting of water containing 10 mM ammonium formate and methanol. This confirmatory method was validated according to EU requirements. Evaluated validation parameters included specificity, accuracy, precision (repeatability and within-laboratory reproducibility), analytical limits (decision limit and detection limit), and applicability. Most parameters were proved to be conforming to the EU requirements. The decision limit (CCα) and detection capability (CCβ) for all analytes ranged from 15.84 to 17.96 μgkg -1. The limit of detection (LOD) and the limit of quantification (LOQ) for all analytes were 0.07 μgkg -1 and 0.2 μgkg -1, respectively. The developed method was successfully applied to monitoring samples collected from the markets in major cities and proven great potential to be used as a regulatory tool to determine mebendazole residues in animal based foods.

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          Multi-residue determination of veterinary drugs in milk by ultra-high-pressure liquid chromatography-tandem mass spectrometry.

          A simple, selective and fast multi-residue method was developed to determine 18 veterinary drugs in milk by ultra-high-pressure liquid chromatography coupled to tandem quadrupole mass spectrometry. The selected antibiotics include quinolones, sulphonamides, macrolides, anthelmintics and one tetracycline. An extraction procedure based on QuEChERS methodology (quick, easy, cheap, effective, rugged and safe), consisting of a liquid extraction of the milk samples with acetonitrile without sample clean up was performed. The extract was centrifuged and the supernatant was filtered prior to chromatographic analysis. Several chromatographic conditions were optimized in order to obtain a fast separation (less than 10 min). The antibiotics were detected by electrospray ionization in positive ion mode with multiple reaction monitoring (MRM) and mass spectrometric conditions were optimized in order to increase selectivity and sensitivity. The developed method was validated in terms of linearity, trueness, precision, limits of detection (LODs) and quantification. Mean recoveries ranged from 70% to 110% and interday precision was lower than 21%. LODs ranged from 1 to 4 microg/kg. Finally, the method was applied to real samples and only traces of tylosin and fenbendezol were detected in two samples.
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            Development and validation of a stability-indicating RP-HPLC method for the determination of paracetamol with dantrolene or/and cetirizine and pseudoephedrine in two pharmaceutical dosage forms.

            A stability-indicating reversed-phase high-performance liquid chromatography (RP-HPLC) method has been developed which can separate and accurately quantitate paracetamol, dantrolene, cetirizine and pseudoephedrine. The method was successfully validated for the purpose of conducting stability studies of the four analytes in quality control (QC) laboratories. The stability-indicating capability of the method was demonstrated by adequate separation of these four analytes from all the degradant peaks. A gradient mobile phase system consisting of (A) 50 mmol L(-1) sodium dihydrogen phosphate, 5 mmol L(-1) heptane sulfonic acid sodium salt, pH 4.2 and (B) acetonitrile was used with Discovery reversed-phase HS C(18) analytical column (250 mm x 4.6 mm i.d., 5 microm particle size). Quantitation was achieved with UV detection at 214 nm, based on peak area. The proposed method was validated and successfully applied for the analysis of pharmaceutical formulations and laboratory-prepared mixtures containing the two multicomponent combinations.
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              Determination of benzimidazoles and levamisole residues in milk by liquid chromatography-mass spectrometry: screening method development and validation.

              The screening method for the determination of residues of 19 benzimidazoles (parent drugs and their metabolites) and levamisole in bovine milk has been developed and validated. Milk samples were extracted with ethyl acetate, sample extracts were cleaned up by liquid-liquid partitioning with hexane and acidic ethanol. Liquid chromatography-single-quadrupole mass spectrometry was used for the separation and determination of analytes. The method was validated in bovine milk, according to the CD 2002/657/EC criteria. An alternative approach to the validation of the method was applied ("sum MRL" substances). The method was successfully verified in CRL proficiency test.
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                Author and article information

                Contributors
                Role: Editor
                Journal
                PLoS One
                PLoS ONE
                plos
                plosone
                PLoS ONE
                Public Library of Science (San Francisco, CA USA )
                1932-6203
                13 January 2017
                2017
                : 12
                : 1
                : e0169597
                Affiliations
                [1 ]Imported Food Analysis Division, Seoul Regional Food and Drug Administration, 212 Mokdongjungang-ro, Yangcheon-Gu, Seoul, Republic of Korea
                [2 ]Department of Biotechnology, College of Life Sciences and Biotechnology, Korea University, 5-Ka, Anam-Dong, Sungbuk-Gu, Seoul, Republic of Korea
                [3 ]Korea Health Supplements Association Sub. Korea Health Supplements Institute, B-dong 101, 700 Daewangpangyo-ro, Bundang-Gu, Seongnam-si, Gyeonggi-do, Republic of Korea
                [4 ]Ministry of Food and Drug Safety, 187 Osongsaengmyeong2(i)-ro, Osong-eup, Heungdeok-gu, Chungju-si, Chungcheonbuk-do, Republic of Korea
                [5 ]Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, 187 Osongsaengmyeong2(i)-ro, Osong-eup, Heungdeok-gu, Chungju-si, Chungcheonbuk-do, Republic of Korea
                [6 ]College of Animal Bioscience and Technology, Department of Bioindustrial Technologies, Konkuk University, Hwayang-dong, Kwangjin-gu, Seoul, Korea
                [7 ]Department of Packaging Science, Clemson University, Clemson, SC, United States of America
                Indian Institute of Science, INDIA
                Author notes

                Competing Interests: The authors have declared that no competing interests exist.

                • Conceptualization: JSL HB HJP.

                • Data curation: JSL SHC CML MIC HJJ HB HJP.

                • Formal analysis: JSL SHC CML MIC HJJ HB HJP.

                • Funding acquisition: HB HJP.

                • Investigation: JSL SHC CML MIC HJJ HB HJP.

                • Methodology: JSL SHC CML MIC HJJ HB HJP.

                • Project administration: JSL HB HJP.

                • Resources: JSL HB HJP.

                • Software: JSL SHC CML MIC HJJ HB HJP.

                • Supervision: JSL HB HJP.

                • Validation: JSL SHC CML MIC HJJ HB HJP.

                • Visualization: JSL SHC CML MIC HJJ HB HJP.

                • Writing – original draft: JSL SHC CML MIC HJJ HB HJP.

                • Writing – review & editing: JSL SHC CML MIC HJJ HB HJP.

                Author information
                http://orcid.org/0000-0003-3057-4999
                Article
                PONE-D-16-31170
                10.1371/journal.pone.0169597
                5234820
                28085912
                9c9a47b8-34cc-40fe-8bce-3498bb109768
                © 2017 Lee et al

                This is an open access article distributed under the terms of the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original author and source are credited.

                History
                : 16 August 2016
                : 25 November 2016
                Page count
                Figures: 5, Tables: 7, Pages: 13
                Funding
                Funded by: Korea Ministry of Food and Drug Safety
                Award ID: No.13161foodsafety002
                Award Recipient :
                This work was supported by a Project (No.13161foodsafety002) for Method development and monitoring on Residues of Veterinary Drugs in foods funded by the Ministry of Food and Drug Safety, Republic of Korea. The funder had no role in study design, data collection and analysis, decision to publish, or preparation of the manuscript.
                Categories
                Research Article
                Biology and Life Sciences
                Agriculture
                Animal Products
                Meat
                Pork
                Biology and Life Sciences
                Nutrition
                Diet
                Food
                Meat
                Pork
                Medicine and Health Sciences
                Nutrition
                Diet
                Food
                Meat
                Pork
                Biology and Life Sciences
                Organisms
                Animals
                Vertebrates
                Amniotes
                Birds
                Fowl
                Gamefowl
                Chickens
                Biology and Life Sciences
                Organisms
                Animals
                Vertebrates
                Amniotes
                Birds
                Poultry
                Chickens
                Biology and Life Sciences
                Agriculture
                Livestock
                Poultry
                Chickens
                Biology and Life Sciences
                Organisms
                Animals
                Vertebrates
                Amniotes
                Mammals
                Equines
                Horses
                Biology and Life Sciences
                Biochemistry
                Metabolism
                Metabolites
                Physical Sciences
                Chemistry
                Chemical Compounds
                Formates
                Physical Sciences
                Chemistry
                Chemical Compounds
                Acids
                Carboxylic Acids
                Formic Acid
                Physical Sciences
                Chemistry
                Chemical Compounds
                Organic Compounds
                Carboxylic Acids
                Formic Acid
                Physical Sciences
                Chemistry
                Organic Chemistry
                Organic Compounds
                Carboxylic Acids
                Formic Acid
                Medicine and Health Sciences
                Pharmacology
                Pharmacokinetics
                Drug Metabolism
                Physical Sciences
                Chemistry
                Chemical Compounds
                Organic Compounds
                Benzimidazoles
                Physical Sciences
                Chemistry
                Organic Chemistry
                Organic Compounds
                Benzimidazoles
                Custom metadata
                All relevant data are within the paper and its Supporting Information files.

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