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

详细信息    查看全文

• 作者：Dan Zhang^a ; Jin-A. Park^a ; Seong-Kwan Kim^a ; Sang-Hyun Cho^a ; Daun Jeong^a ; Soo-Min Cho^a ; Hee Yi^a ; Jae-Han Shim^b ; Jin-Suk Kim^a ; A.M. Abd El-Aty^a ; ^c ; ^{abdelaty44@hotmail.com" class="auth_mail" title="E-mail the corresponding author} ; ^{amabdelaty@konkuk.ac.kr" class="auth_mail" title="E-mail the corresponding author} ; Ho-Chul Shin^a ; ^{hshin@konkuk.ac.kr" class="auth_mail" title="E-mail the corresponding author}
• 关键词：Flumethasone ; dl-Methylephedrine ; 2-Hydroxy-4 ; 6-dimethylpyrimidine ; Tandem mass spectrometry ; Porcine muscle ; Milk ; Veterinary drugs
• 刊名：Journal of Chromatography B, Analytical Technologies in the Biomedical and Life Sciences
• 出版年：2016
• 出版时间：15 February 2016
• 年：2016
• 卷：1012-1013
• 期：Complete
• 页码：8-16
• 全文大小：1151 K

文摘

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 10 mM 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 10 mM ammonium formate in ultrapure water and acetonitrile. Good linearity was achieved over the tested concentrations in matrix-fortified calibrations with correlation coefficients (R²) ≥ 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 2–10 ng/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.