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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 被引量:13

Determination of 9 Steroid Hormones in Pork and Beef Samples by Filtration Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
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摘要 建立通过式固相萃取-超高效液相色谱-串联质谱法检测猪肉和牛肉中9种类固醇激素的方法。样品于37℃酶解16 h,乙腈涡旋提取后,经新型PRiME HLB通过式固相萃取小柱净化,采用Waters Acquity BEH C18色谱柱(2.1 mm×100 mm,2.5μm)分离,以体积分数0.1%甲酸水溶液-乙腈为流动相进行梯度洗脱,使用电喷雾离子源正离子模式检测,内标法定量。结果表明:9种类固醇激素在0.2~100.0 ng/mL质量浓度范围内线性关系良好,检出限为0.2~0.5μg/kg,定量限为0.4~1.0μg/kg;方法回收率为84.5%~117.3%,相对标准偏差小于10%。该方法操作简便且灵敏度高,适用于猪肉和牛肉中9种类固醇激素的定量分析。 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,2.5μm)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 0.4–1.0μg/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.
作者 张再永 马俊美 李强 范斌 刘亮 ZHANG Zaiyong;MA Junmei;LI Qiang;FAN Bin;LIU Liang(Technical Evaluation Center of Hebei Administration for Market Regulation,Shijiazhuang 050091,China;Key Laboratory of Food Safety of Hebei Province,Hebei Food Inspection and Research Institute,Shijiazhuang 050227,China)
出处 《肉类研究》 北大核心 2020年第7期58-63,共6页 Meat Research
基金 河北省市场监督管理局科技计划项目(2020ZD06)。
关键词 通过式固相萃取 超高效液相色谱-串联质谱法 类固醇激素 内标法 filtration solid phase extraction ultra performance liquid chromatography-tandem mass spectrometry steroid hormones internal standard method
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