title: Simultaneous detection of flumethasone, dl-methylephedrine, and 2-hydroxy-4,6-dimethylpyrimidine in porcine muscle and pasteurized cow milk using liquid chromatography coupled with triple-quadrupole mass spectrometry.
abstract: A simple analytical method based on liquid chromatography coupled with triple-quadrupole mass spectrometry was developed for detection of the veterinary drugs flumethasone, dl-methylephedrine, and 2-hydroxy-4,6-dimethylpyrimidine in porcine muscle and pasteurized cow milk. The target drugs were extracted from samples using 10mM ammonium formate in acetonitrile followed by clean-up with n-hexane and primary secondary amine sorbent (PSA). The analytes were separated on an XBridge™ hydrophilic interaction liquid chromatography (HILIC) column using 10mM ammonium formate in ultrapure water and acetonitrile. Good linearity was achieved over the tested concentrations in matrix-fortified calibrations with correlation coefficients (R(2))≥0.9686. Recovery at two spiking levels ranged between 73.62-112.70% with intra- and inter-day precisions of ≤20.33%. The limits of quantification ranged from 2-10ng/g in porcine muscle and pasteurized cow milk. A survey of market samples showed that none of them contained any of the target analytes. Liquid-liquid purification using n-hexane in combination with PSA efficiently removed the interferences during porcine and milk sample extraction. The developed method is sensitive and reliable for detection of the three target drugs in a single chromatographic run. Furthermore, it exhibits high selectivity and low quantification limits for animal-derived food products destined for human consumption.
authors.affiliation: Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul 143-701, Republic of Korea.
authors.forename: Dan
authors.initials: D
authors.lastname: Zhang
authors.affiliation: Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul 143-701, Republic of Korea.
authors.forename: Jin-A
authors.initials: JA
authors.lastname: Park
authors.affiliation: Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul 143-701, Republic of Korea.
authors.forename: Seong-Kwan
authors.initials: SK
authors.lastname: Kim
authors.affiliation: Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul 143-701, Republic of Korea.
authors.forename: Sang-Hyun
authors.initials: SH
authors.lastname: Cho
authors.affiliation: Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul 143-701, Republic of Korea.
authors.forename: Daun
authors.initials: D
authors.lastname: Jeong
authors.affiliation: Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul 143-701, Republic of Korea.
authors.forename: Soo-Min
authors.initials: SM
authors.lastname: Cho
authors.affiliation: Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul 143-701, Republic of Korea.
authors.forename: Hee
authors.initials: H
authors.lastname: Yi
authors.affiliation: Biotechnology Research Institute, College of Agriculture and Life Sciences, Chonnam National University, 300 Yongbong-dong, Buk-gu, Gwangju 500-757, Republic of Korea.
authors.forename: Jae-Han
authors.initials: JH
authors.lastname: Shim
authors.affiliation: Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul 143-701, Republic of Korea.
authors.forename: Jin-Suk
authors.initials: JS
authors.lastname: Kim
authors.affiliation: Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul 143-701, Republic of Korea; Department of Pharmacology, Faculty of Veterinary Medicine, Cairo University, 12211 Giza, Egypt. Electronic address: abdelaty44@hotmail.com.
authors.forename: A M
authors.initials: AM
authors.lastname: Abd El-Aty
authors.affiliation: Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul 143-701, Republic of Korea. Electronic address: hshin@konkuk.ac.kr.
authors.forename: Ho-Chul
authors.initials: HC
authors.lastname: Shin
mesh_terms: D000818:Animals; D002417:Cattle; D002853:Chromatography, Liquid / Q000379:methods*; D004809:Ephedrine / Q000031:analogs & derivatives* / Q000032:analysis; D005443:Flumethasone / Q000032:analysis*; D008460:Meat / Q000032:analysis; D008892:Milk / Q000737:chemistry*; D018482:Muscle, Skeletal / Q000737:chemistry*; D011744:Pyrimidinones / Q000032:analysis*; D013552:Swine; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D011744:Pyrimidinones; C044189:2-hydroxy-4,6-dimethylpyrimidine; C041707:N-methylephedrine; D004809:Ephedrine; D005443:Flumethasone
keywords: 2-Hydroxy-4,6-dimethylpyrimidine; Flumethasone; Milk; Porcine muscle; Tandem mass spectrometry; Veterinary drugs; dl-Methylephedrine