分散固相萃取-同位素稀释-高效液相色谱-串联质谱法同时测定猪肉中26种β-受体激动剂
发布时间：2018-10-31 12:50
【摘要】：建立了分散固相萃取-同位素稀释-高效液相色谱-串联质谱(dSPE-ID-HPLC-MS/MS)同时测定猪肉中26种β-受体激动剂残留的方法。样品经β-葡萄糖醛苷酶/芳基硫酸酯酶水解12 h后,用高氯酸沉淀蛋白质,取上清液,调节pH值为9,用乙腈涡旋提取,分散固相萃取净化。选用具有混合分离模式的新型色谱柱Poroshell 120Phenyl-Hexyl(100 mm×2.1 mm,4.0μm)对待测物进行分离,在电喷雾离子(ESI)源正离子模式下以多反应监测(MRM)模式采集数据并做定性筛查和定量分析。26种待测物在相应的浓度范围内线性关系良好,相关系数均大于0.99,在3个不同浓度的添加水平下,平均回收率为65.3%~108.5%,相对标准偏差(RSD)为2.7%~13.3%,检出限(LOD,S/N=3)和定量限(LOQ,S/N=10)分别为0.03~0.1μg/kg及0.1~1.0μg/kg。该方法成本低廉、灵敏可靠,适用于同时对猪肉产品中26种β-受体激动剂残留进行定性和定量筛查。
[Abstract]:A method for simultaneous determination of 26 尾 -agonist residues in pork by dispersive solid-phase extraction, isotope dilution, high performance liquid chromatography-tandem mass spectrometry (dSPE-ID-HPLC-MS/MS) was developed. The sample was hydrolyzed by 尾 -glucuronidase / aryl sulfate for 12 h, then the protein was precipitated with perchloric acid, the supernatant was extracted, the pH value was adjusted to 9, extracted by acetonitrile vortex, and purified by dispersive solid-phase extraction. A new Poroshell 120Phenyl-Hexyl (100 mm 脳 2. 1 mm,4.0 渭 m) column with mixed separation mode was used to separate the determination. In the positive ion mode of electrospray ion (ESI) source, the data were collected by multi-reaction monitoring (MRM) mode, and the qualitative screening and quantitative analysis were done. The linear relationship of 26 kinds of samples was good in the corresponding concentration range, and the correlation coefficients were all greater than 0.99. At three different concentration levels, the average recovery rate was 65.3% and 108.5%, and the relative standard deviation (RSD) was 2.7and 13.3.The detection limit (LOD,S/N=3) and the quantitative limit (LOQ,) were obtained. The S/N=10 was 0.03 渭 g/kg and 0.1 渭 g / kg, respectively. The method has the advantages of low cost, high sensitivity and reliability. It is suitable for qualitative and quantitative screening of 26 尾-agonist residues in pork products at the same time.
【作者单位】： 中国广州分析测试中心广东省分析测试技术公共实验室;
【基金】：广东省科技计划项目(2014B070705001) 广州市科技计划项目(11BppZXcc6100034)~~
【分类号】：O657.63;TS251.7
[Abstract]:A method for simultaneous determination of 26 尾 -agonist residues in pork by dispersive solid-phase extraction, isotope dilution, high performance liquid chromatography-tandem mass spectrometry (dSPE-ID-HPLC-MS/MS) was developed. The sample was hydrolyzed by 尾 -glucuronidase / aryl sulfate for 12 h, then the protein was precipitated with perchloric acid, the supernatant was extracted, the pH value was adjusted to 9, extracted by acetonitrile vortex, and purified by dispersive solid-phase extraction. A new Poroshell 120Phenyl-Hexyl (100 mm 脳 2. 1 mm,4.0 渭 m) column with mixed separation mode was used to separate the determination. In the positive ion mode of electrospray ion (ESI) source, the data were collected by multi-reaction monitoring (MRM) mode, and the qualitative screening and quantitative analysis were done. The linear relationship of 26 kinds of samples was good in the corresponding concentration range, and the correlation coefficients were all greater than 0.99. At three different concentration levels, the average recovery rate was 65.3% and 108.5%, and the relative standard deviation (RSD) was 2.7and 13.3.The detection limit (LOD,S/N=3) and the quantitative limit (LOQ,) were obtained. The S/N=10 was 0.03 渭 g/kg and 0.1 渭 g / kg, respectively. The method has the advantages of low cost, high sensitivity and reliability. It is suitable for qualitative and quantitative screening of 26 尾-agonist residues in pork products at the same time.
【作者单位】： 中国广州分析测试中心广东省分析测试技术公共实验室;
【基金】：广东省科技计划项目(2014B070705001) 广州市科技计划项目(11BppZXcc6100034)~~
【分类号】：O657.63;TS251.7
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1 张学亮;罗云敬;姜洁;路勇;冯楠;;分子印迹固相萃取-超高效液相色谱-串联质谱法测定猪肉中5种β_2-受体激动剂残留[J];色谱;2015年08期
2 刘佳;谢云峰;任丹丹;崔兴品;梁桂荣;杨永坛;;反相液相色谱-串联质谱法检测猪肝中26种β_2-受体激动剂类药物残留[J];分析化学;2014年10期
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