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Simultaneous Determination of Phenobarbital, Pentobarbital, Amobarbital and Secobarbital in Raw Milk via Liquid Chromatography with Electron Spray Ionization Tandem Mass Spectrometry
Korean J. Food Sci. An. 2017;37:847-854
Published online December 31, 2017
© 2017 Korean Society for Food Science of Animal Resources

Huaixiang Tian1, Xingxin Zhou1, Chen Chen1, Yabin He, Haiyan Yu1, and Xiaoping Zheng*

Shanghai Bino Testing Technology Service, Shanghai, China
1School of Perfume and Aroma Technology, Shanghai Institute of Technology, Shanghai 200436, China
Correspondence to: Xiaoping Zheng
Shanghai Bino Testing Technology Service, 1577 West Jiangchang Rd, Shanghai 200436, China
Tel: +86-21-55155277 Fax: +86-21-55156873 E-mail: 13917009499@163.com
Received September 4, 2017; Revised November 1, 2017; Accepted November 2, 2017.
This is an Open Access article distributed under the terms of the Creative Commons Attribution Non-Commercial License (http://creativecommons.org/licenses/by-nc/3.0) which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original work is properly cited.
Abstract
A rapid, sensitive and specific liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the simultaneous determination of four barbiturates (phenobarbital, pentobarbital, amobarbital and secobarbital) in raw milk. The barbiturates were extracted using liquid-liquid extraction, ultrasonication and centrifugation, and purified on an SPE column. Analytes were separated by HPLC on a CSH C18 column eluted using an acetonitrile- water system with a linear gradient dilution programme, and detected by MS/MS. The recoveries of the barbiturates were 85.0-113.5%, and the intra- and inter-assay RSDs were less than 9.8% and 7.3%, respectively. The limit of detection was 5 ng/mL for all four of the barbiturates. The analytical method exhibited good linearity from 10 to 1000 ng/mL; the correlation coefficient (r2) was greater than 0.9950 for each barbiturate. This method was also applied to the determination of barbiturates in real milk samples and was found to be suitable for the determination of veterinary drug residues in raw milk.
Keywords : barbiturates, raw milk, veterinary drug residue, LC-MS/MS


June 2018, 38 (3)