超高效液相色谱-高分辨谱法同时测定牛肉中的苯基丁氮酮和氨基比林  

Determination of Phenylbutazone and Aminopyrine in Beef by Ultra High Performance Liquid Chromatography-High Resolution Mass Spectrometry

作　　者：张海燕[1] 刘鑫[2] 严华[2] 李建辉[2] 张朝晖[2] 卢晓宇[2] 张沫琦 李岩[2] 叶晓霞[1] 

机构地区：[1]温州医科大学药学院,浙江温州325035 [2]北京出入境检验检疫局,北京100026

出　　处：《食品科学》2013年第24期135-139,共5页Food Science

基　　金：国家质检行业公益性科研专项(201210029);国家质检总局科研计划项目(2012IK145;2013IK146)

摘　　要：建立超高效液相色谱．高分辨质谱法（UPLC-HRMS）同时测定动物源食品中苯基丁氮酮和氨基比林的分析方法。样品前处理使用改进的QuEChERS方法，考察多种溶剂体系，最终选择丙酮和水作为提取溶剂，AcquityUPLCHSST3色谱柱（150mm×2．1mm，1．8μm）分离，以乙腈和乙酸铵溶液作为流动相进行梯度洗脱，电喷雾正离子（EST＋）模式，全扫描模式进行检测。结果表明：苯基丁氮酮在5．0～100．0μg／L范围内线性关系良好（r≥0．995），氨基比林在1．0～100．0μg／L范围内线性关系良好（r≥0．995）。牛肉中两种非甾体类阵痛药都有较好的回收率和稳定性：5．0、10．0、20．0μg／kg的添加水平的回收率为76．7％-85．9％，相对标准偏差（RSD，n=6）为5．6％-12．9％。苯基丁氮酮和氨基比林的定量限（RSN=10）分别为5．0μg／kg和1．0gg／kg。该方法简单、快速、灵敏、准确，适合于动物源食品中苯基丁氮酮和氨基比林等非甾体类镇痛剂的快速、高灵敏的分析检测。A method for the determination of phenylbutazone and aminopyrine in beef has been developed by ultra high perfor- mance liquid chromatography-high resolution mass spectrometry （UHPLC-HRMS）. After a modified QuEChRES sample prepara- tion process, the samples were loaded onto an Acquity UPLC HSS T3 column （150 mm × 2.1 mm, 1.8 μm） and separated with a gradient elution. The electrospray process was operated in the positive ion mode, and data were acquired in the full scan mode. The calibration curves showed a good linearity in the range of 5.0-100.0 μ/kg, with correlation coefficients （r） equal to or greater than 0.995. When the spiked levels were 5, 10 μg/kg and 20 μg/kg, the recovery rates of phenylbutazone and arninopyrine in bovine ranged from 76.7% to 85.9%, with relative standard deviations （RSDs） of 5.6%-12.9%. The limits of quantification （LOQs, RsN=10） for phenylbutazone and aminopyrine were 5.0 μg/kg and 1.0 μg/kg in beef, respectively. The results indicate that the developed method is simple, rapid, sensitive and suitable for the qualitative and quantitative analysis of phenylbutazone and aminopyrine in animal-derived foodstuffs including beef.

关 键 词：超高效液相色谱 高分辨质谱法 苯基丁氮酮 氨基比林 牛肉 

分 类 号：O657[理学—分析化学]