超高效液相色谱-串联质谱法同时测定牛奶中 25 种兽药的多残留分析
Multiclass analysis of 25 veterinary drugs in milk by ultra-high performance liquid chromatography-tandem mass spectrometry.
机构信息
Institute of Drug Discovery & Development, School of Pharmaceutical Sciences, Zhengzhou University, Henan Province, Zhengzhou 450001, China; Key Laboratory of Advanced Drug Preparation Technologies, Ministry of Education, Zhengzhou University, Henan Province, Zhengzhou 450001, China; Collaborative Innovation Center of New Drug Research and Safety Evaluation, Henan Province, Zhengzhou 450001, China.
Institute of Drug Discovery & Development, School of Pharmaceutical Sciences, Zhengzhou University, Henan Province, Zhengzhou 450001, China.
出版信息
Food Chem. 2018 Aug 15;257:259-264. doi: 10.1016/j.foodchem.2018.02.144. Epub 2018 Feb 28.
The aim of this work was to develop a simple and rapid analytical method for the simultaneous determination of a wide range of drug residues in milk by UHPLC-MS/MS. A total of 25 typical veterinary drugs investigated belong to six families including β-lactams, quinolones, β-agonists, phenicols, glucocorticoids and nitrofurans. The samples were extracted by acetonitrile and defatted with n-hexane twice. Electrospray ionization and positive/negative polarity switching were utilized for the analysis of 25 veterinary drugs in a single chromatographic run. The linearity, recovery, precision and matrix effects of the method were fully validated. The intra- and inter-precision were in the range of 1.7-11.1% and 2.5-10.4%, respectively. The average recoveries ranged from 65.9% to 123.5% with RSD less than 10.8% at three concentration levels. The proposed method was demonstrated to be simple, economical and reliable for the fast monitoring of these drug residues in milk samples.
本工作旨在建立一种简单、快速的超高效液相色谱-串联质谱法（UHPLC-MS/MS），用于同时检测牛奶中多种药物残留。共选择了 25 种典型的兽药，分属于β-内酰胺类、喹诺酮类、β-激动剂类、苯氧酰胺类、糖皮质激素类和硝基呋喃类 6 个家族。样品用乙腈提取，正己烷脱脂 2 次。采用电喷雾离子源，正、负离子切换模式，在单次色谱运行中分析 25 种兽药。该方法对线性、回收率、精密度和基质效应进行了全面验证。方法的日内和日间精密度分别在 1.7%11.1%和 2.5%10.4%范围内，3 个浓度水平的平均回收率在 65.9%~123.5%之间，相对标准偏差（RSD）均小于 10.8%。该方法简单、经济、可靠，可用于快速监测牛奶中这些药物残留。
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