Determination of 9 Steroid Hormones in Pork and Beef Samples by Filtration Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
ZHANG Zaiyong, MA Junmei, LI Qiang, FAN Bin, LIU Liang
1.Technical Evaluation Center of Hebei Administration for Market Regulation, Shijiazhuang 050091, China; 2.Key Laboratory of Food Safety of Hebei Province, Hebei Food Inspection and Research Institute, Shijiazhuang 050227, China
Abstract:A method for determination of 9 steroid hormones in pork and beef was developed by filtration solid phase extraction (FSPE) followed by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Samples were digested for 16 h at 37 ℃, extracted with acetonitrile, and purified by a PRiME HLB cartridge. Then the analytes were separated on a Waters Acquity BEH C18 column (2.1 mm × 100 mm,2.5 μm) by gradient elution using a mixture of 0.1% formic acid solution and acetonitrile as the mobile phase. The detection was operated using an electrospray ionization source in the positive mode, and quantitation was performed by the internal standard method. The results showed that the nine steroid hormones had a good linear relationship in the concentration range of 0.2–100.0 ng/mL. The limits of detection and limits of quantitation were respectively 0.2–0.5 and 0.4–1.0 μg/kg. Recoveries of the method were in the range of 84.5%–117.3%, with relative standard deviation (RSD) lower than 10%. The method is simple, sensitive, and useful for quantification of 9 steroid hormones in pork and beef samples.
张再永,马俊美,李 强,范 斌,刘 亮. 通过式固相萃取-超高效液相色谱-串联质谱法测定猪肉和牛肉中9种类固醇激素[J]. 肉类研究, 2020, 34(7): 58-63.
ZHANG Zaiyong, MA Junmei, LI Qiang, FAN Bin, LIU Liang. Determination of 9 Steroid Hormones in Pork and Beef Samples by Filtration Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry. Meat Research, 2020, 34(7): 58-63.