蛋及蛋制品中多药物残留快速检测技术研究

Studies of rapid determination for multi-residues of drugs in eggs and egg products

中文关键词:  蛋及蛋制品  多类药物残留  QuEChERS  超高效液相色谱-四极杆-飞行时间质谱法  高分辨质谱数据库

英文关键词:eggs and egg products  multi-residues of drugs  QuEChERS  ultra performance liquid chromatography-quadrupole-time of flight-mass spectrometry  accurate mass database

中文摘要:

      目的 建立蛋及蛋制品中5类49种药物残留的QuEChERS方法并应用超高效液相色谱-四极杆-飞行时间质谱(ultra performance liquid chromatography-quadrupole-time of flight-mass spectrometry, UPLC-Q-TOF- MS)高分辨质谱数据库快速定性筛查确证及参考定量。方法 采用5 mL 5%甲酸乙腈溶液提取, C18与PSA吸附剂净化的QuEChERS方法进行前处理, 经Waters ACQUITY UPLC BEH C18(2.1 mm×50 mm, 1.7 μm)色谱柱分离, 以5 mmol/L乙酸铵溶液(含0.1%甲酸)-乙腈为流动相, 梯度洗脱, Q-TOF-MS电喷雾正、负离子模式检测, 通过Waters Masslynx工作站的Chromalynx XS模块建立多种药物的精确质量数和全扫描碰撞诱导解离碎片离子高分辨质谱数据库。结果 49种药物呈现良好的线性关系, 相关系数均大于0.99, 检出限(S/N＝3)为0.2~10 μg/kg, 回收率结果在69.4%~121.5%之间。结论 该方法简便、快速、灵敏, 适用于蛋及蛋制品中多类药物残留的同时检测。

英文摘要:

      Objective To establish a method for the rapid qualitative screening and reference quantification of 5 kinds of 49 kinds of drug residues in eggs and egg products by QuEChERS-ultra performance liquid chromatography-quadrupole-time of flight-mass spectrometry (UPLC-Q-TOF-MS) high resolution mass spectrometry database. Methods The sample was extracted by 5 mL 5% formic acid acetonitrile solution, The pretreatment was performed with QuEChERS method purified by C18 and PSA adsorbent, and the sample was separated by Waters ACQUITY UPLC BEH C18 (2.1 mm×50 mm, 1.7 μm) column. Using 5 mmol/L ammonium acetate solution (containing 0.1% formic acid) - acetonitrile as mobile phase, gradient elution, q-tof -MS electrospray positive and negative ion mode detection The accurate mass number and full scanning collision induced dissociation fragment ion high resolution mass spectrometry database was established by Chromalynx XS module of Waters Masslynx workstation. Results The correlation coefficients were all greater than 0.99, the detection limits (S/N=3) were 0.2?10 g/kg, and the recoveries were 69.4%?121.5%. Conclusion This method is simple, rapid and sensitive, and is suitable for simultaneous detection of various drug residues in eggs and egg products.