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食品研究与开发:2025,46(2):194-200
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基于固相萃取-超高效液相色谱-串联质谱法测定畜禽肉中3 种青霉素类的残留量
(郑州市产品质量检验检测中心,河南 郑州 450006)
Determination of Three Penicillin Residues in Meat by Solid Phase Extraction-Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry
(Product Quality Inspection and Testing Center of Zhengzhou,Zhengzhou 450006,Henan,China)
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投稿时间:2023-12-28    
中文摘要: 为测定畜禽肉中苄青霉素、邻氯青霉素和氨苄青霉素3 种青霉素的残留量,该文建立固相萃取-超高效液相色谱-串联质谱(solid phase extraction-ultra-high performance liquid chromatography-mass spectrometry/mass spectrometry,SPE-UPLC-MS/MS)法同时测定畜禽肉中3 种青霉素残留量的分析方法。对影响固相萃取柱效率的洗脱剂的种类、洗脱剂用量以及上样速率进行优化;同时对样品的提取和净化条件进行考察。在3 mL/min 的上样速率下,用6 mL乙腈洗脱可达到最佳的萃取效果。以0.1% 甲酸水溶液-乙腈作为流动相进行梯度洗脱,在UPLC C18 色谱柱上分离,电喷雾正离子模式下,以动态多反应监测采集数据,外标法定量。3 种目标分析物的线性回归方程相关系数均大于0.999,检出限为0.05~0.10 μg/kg(信噪比S/N=3),定量限为0.1~0.4 μg/kg(S/N=10),加标回收率为82.7%~96.8%,相对标准偏差为1.92%~4.61%。SPE-UPLC-MS/MS 方法具有精密度高、重复性好、分离度高、分析时间短等优点,可适用于畜禽肉中青霉素定性定量测定。
Abstract:A method for determining the residues of benzylpenicillin,cloxacillin,and ampicillin in meat was established based on solid phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS). The main factors affecting the efficiency of solid phase extraction,such as the type and volume of eluent and sample loading rate,were optimized. At the same time,the extraction and purification conditions of samples were investigated. The optimal purification effect was achieved at the sample flow rate of 3 mL/min with 6 mL acetonitrile. The HPLC separation was carried out in a UPLC C18 column with 0.1% formic acid aqueous solution-acetonitrile as the mobile phase for gradient elution. The data were collected by dynamic multiple reaction monitoring (MRM) in positive ion mode (electrospray ionization) and quantified by the external standard method. The correlation coefficients of the linear regression equations of the three target analytes were all greater than 0.999,and the limits of detection (S/N=3) and quantification (S/N=10) ranged from 0.05 to 0.10 μg/kg and from 0.1 to 0.4 μg/kg,respectively. The average recovery of the 3 analytes varied within 82.7%-96.8% and the relative standard deviations were within 1.92%-4.61%. With high precision,high reproducibility,high resolution,and short analysis time,the established SPE-UPLC-MS/MS method is suitable for qualitative and quantitative determination of penicillins in meat.
文章编号:202502025     中图分类号:    文献标志码:
基金项目:河南省市场监督管理局科技计划项目(2022sj129、2022sj134)
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