Citation: LUO Huitai, HUANG Xiaolan, WU Huiqin, ZHU Zhixin, HUANG Fang, LIN Xiaoshan, ZHANG Qiuyan, MA Yefen. Simultaneous determination of 26 β-agonists in pork by dispersive solid-phase extraction and isotope dilution-high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2016, 34(5): 481-489. doi: 10.3724/SP.J.1123.2016.01015 shu

Simultaneous determination of 26 β-agonists in pork by dispersive solid-phase extraction and isotope dilution-high performance liquid chromatography-tandem mass spectrometry

1.
China National Analytical Center(Guangzhou), Guangdong Provincial Public Laboratory of Analysis and Testing Technology, Guangzhou 510070, China

Corresponding author: HUANG Xiaolan,
Received Date: 12 January 2016

Fund Project: 广东省科技计划项目(2014B070705001) (2014B070705001)广州市科技计划项目(11BppZXcc6100034). (11BppZXcc6100034)

A method has been developed and validated for the determination of 26 β-agonists in pork using dispersive solid-phase extraction (dSPE) coupled with isotope dilution-high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). After the samples were hydrolyzed by β-glucuronidase/aryl sulfatase for 12 h, the protein was precipitated with perchloric acid. The analytes were extracted with vortex mixer by acetonitrile after adjusting the pH value to nine, and then the extracts were purified using mixed adsorbent by dSPE. After the separation on a novel mixed-mode column of Poroshell 120 Phenyl-Hexyl (100 mm×2.1 mm, 4.0 μ m), the qualitative and quantitative analyses of the 26 analytes were operated by electrospray ionization mass spectrometry in the positive mode using multiple reaction monitoring (MRM). The correlation coefficients of linear calibration curves were over 0.99 in the corresponding concentration ranges. The average recoveries of the 26 β-agonists ranged from 65.3% to 108.5%, and the relative standard deviations (RSDs) were 2.7%-13.3% in spiked sample at three levels. The limits of detection (LODs, S/N=3) and the limits of quantification (LOQs, S/N=10) were 0.03-0.1 μ g/kg and 0.1-1.0 μ g/kg, respectively. The method is low cost, sensitive, reliable and suitable for the determination of residues of the 26 β-agonists in pork products.
- dispersive solid-phase extraction (dSPE),
- isotope dilution,
- high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS),
- β-agonists,
- pork
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