QuEChERS/超高效液相色谱-电喷雾串联质谱法检测鸡肉中11种激素类药物残留  

Determination of 11 hormones residues in chicken using QuEChERS sample preparation method with ultra performance liquid chromatography-tandem mass spectrometry

作　　者：连英杰 林升航 曾琪[1] 吴敏[1] 徐敦明[1] 林立毅[1] 周昱[1] 黄志强 

机构地区：[1]厦门出入境检验检疫局,厦门361000 [2]湖南省检验检疫科学技术研究院,长沙410004

出　　处：《食品安全质量检测学报》2014年第2期384-392,共9页Journal of Food Safety and Quality

基　　金：国家科技支撑计划项目(2012BAK08B01)~~

摘　　要：目的：建立鸡肉中4种雄激素,3种孕激素,4种糖皮质激素药物多残留的QuEChERS/超高效液相色谱-串联质谱(ultra pressure liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时测定方法。方法样品用乙酸乙酯提取,经QuEChERS分散固相萃取净化后,采用phenomenex kinetex色谱柱分离,分别在电喷雾正、负离子模式下以多反应监测(multiple reaction monitoring, MRM)方式检测。正、负离子模式下流动相均为0.1%甲酸水和乙腈梯度洗脱。结果11种药物在相应的浓度范围内线性良好,相关系数均大于0.991,在3个加标水平下的平均回收率为84.4%~94.1%,相对标准偏差(RSD)为7.5%~12.5%,检出限(LOD, S/N≥3)和定量下限(LOQ, S/N≥10)分别为0.37~9.55μg/kg及1.11~28.65μg/kg。结论该方法简便快速、灵敏可靠、经济有效,适用于鸡肉中激素类药物多残留的同时快速测定。Objective A multi-residue testing method was developed for the simultaneous determination of 4 androgens, 3 progesterones and 4 glucocorticoids in chicken using QuEChERS sample preparation method with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods The homogenized sample extracted with ethyl acetate. The separation was performed on a phenomenex kinetex column by gradient elution after puring from dispersive-solid-phase extraction(d-SPE). The analysis of 11 ana-lytes were operated by electrospray ionization mass spectrometry under the positive or negative mode using multiple reaction monitoring (MRM). Acetonitrile and water(containing 0.1% formic acid) were used as the mobile phase both in positive and negative. Results The correlation coeficients of calibration curves were over 0.991 in the corresponding concentration range. The average recoveries of the 11 analytes at three spiked concentration levels varied from 84.4%to 94.1%and the relative standard deviations(RSDs) varied from 7.5%to 12.5%. The limits of detection(LOD, S/N≥3) and quantitation(LOQ, S/N≥10) were 0.37~9.55 μg/kg and 1.11~28.65μg/kg, respectively. Conclusion The real sample tests showed that the proposed method was sim-ple, rapid, sensitive, reliable and cost-effective, and it was suitable for the simultaneous determination of hor-mones residues in chicken samples.

关 键 词：QUECHERS 超高效液相色谱-串联质谱 雄激素 孕激素 糖皮质激素 鸡肉 

分 类 号：O657.63[理学—分析化学] TS251.7[理学—化学]