QuEChERS EMR Lipid净化结合同位素稀释-超高效液相色谱-串联质谱法同时测定畜肉中17种β-受体激动剂

Simultaneous Determination of 17β-Receptor Agonists in Meat by QuEChERS EMR-Lipid with Isotope Dilution-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

目的:建立了一种采用QuEChERS EMR Lipid净化结合同位素稀释-超高效液相色谱-串联质谱技术同时测定畜肉中17种β-受体激动剂药物残留的检测方法。方法:样品加入pH为5.2的乙酸铵缓冲溶液,以β-葡萄糖醛苷酶/芳基硫酸酯酶酶解,经5%甲酸乙腈提取,QuEChERS EMR Lipid净化,采用CORTECS^(™)UPLC®C_(18)柱(3.0 mm×100 mm,1.6μm),0.1%甲酸水和甲醇梯度洗脱,在分时段多反应监测(scheduled MRM,sMRM)模式下测定,内标法定量。结果:17种β-受体激动剂在0~20 ng/mL浓度范围内线性相关系数均大于0.99,方法检出限为0.01~0.09μg/kg,定量限为0.05~0.31μg/kg。在0.5、2.0、5.0μg/kg 3个加标浓度水平下的平均回收率为81.7%~111.8%,RSD为0.8%~10.3%(n=6)。100批市售生鲜畜肉中未检出β-受体激动剂。结论:该法前处理步骤简便,净化效果良好,缩短酶解时间,提高了样品检测效率,内标法定量精准可靠,适用于大批量畜肉样品中多种β-受体激动剂药物残留的同时检测。

Objective:A method for simultaneous determination of 17β-receptor agonists in meat was established by QuEChERS EMR-Lipid with isotope dilution-ultra performance liquid chromatography-tandem mass spectrometry.Methods:The samples were added to ammonium acetate buffer solution(pH5.2)and enzymatic hydrolyzed byβ-glucuronidase and arysulfatase.The hydrolysates were extracted by acetonitrile containing 5%formic acid,and purified by QuEChERS EMR-Lipid.The analyses were separated by CORTECS^(™)UPLC®C_(18) chromatographic column with gradient elution using 0.1%formic acid and methanol as the mobile phase.The target compounds were monitored in scheduled MRM mode.Then the internal standard method was used for quantitative analysis.Results:The linear regression correlation coefficients for the 17β-receptor agonists were all higher than 0.99 in the range from 0 ng/mL to 20 ng/mL.The limits of detection were 0.01~0.09μg/kg and the limits of quantification were 0.05~0.31μg/kg.The average recoveries at three spiked levels of 0.5,2.0 and 5.0μg/kg ranged from 81.7%to 111.8%with the relative standard deviations of 0.8%~10.3%(n=6).Noβ-receptor agonists were detected in 100 batches of fresh meat.Conclusion:The method has the advantages of simple pretreatment steps and good purification effect.It shortened enzymolysis time,improved sample detection efficiency.The internal standard method was accurate and reliable.It was suitable for simultaneous determination ofβ-receptor agonists in a large number of meat samples.