空间位阻净化-液相色谱-串联质谱技术测定动物源性食品中抗组胺类药物残留的方法研究

摘要/Abstract

摘要： 建立了超高效液相色谱-串联质谱法（UPLC-MS/MS）快速测定动物源性食品中19种抗组胺类药物及其代谢物残留的方法。样品用乙腈-乙酸乙酯溶液提取，提取液经空间位阻净化吸附剂（EMR）净化，再经无水硫酸镁（MgSO4）和氯化钠（NaCl）盐析并浓缩后测定，以0.1%甲酸水-0.1甲酸乙腈作为流动相进行梯度洗脱，在Poroshell 120 EC-C18（100mm L x 2.1mm ID, 2.7μm）色谱柱上分离，柱温35℃，流速0.3mL/min，进样量10μL，在电喷雾正离子模式下以动态多反应监测（Dynamic MRM）采集数据，外标法定量。结果表明，19种抗组胺类药物及其代谢物在相应浓度范围内线性良好，相关系数均大于0.999，不同阴性样品基质中（牛肉、鸡肉、猪肝）在3个浓度水平加标试验回收率在75.1～89.3% 之间，相对标准偏差（RSD）为2.3～7.5%，方法检测限(LOD，S/N≥3）为0.2～2.0μg/kg，定量限为0.6～6.0μg/kg。经方法学验证，本方法简便快速，重现性好，灵敏度高，结果可靠。适用于动物源性食品中19种抗组胺类药物及其代谢物的快速筛查和定量测定。

关键词: 抗组胺药物, 超高效液相色谱-串联质谱, 动物源食品, EMR-Lipid吸附剂

Abstract: A method for rapid determination of 19 antihistamines and their metabolites in animal derived food by UPLC-MS/MS was established.The sample was extracted by acetonitrile-ethyl acetate solution, the extract was purified by steric barrier purification adsorbent (EMR), and then salted out and concentrated by MgSO4 and NaCl. Data were collected by dynamic multi-reaction monitoring (Dynamic MRM) in electrospray cation mode with a sample size of 10μL, flow rate of 0.3 mL/min, mobile phase of 0.1% water-formic and 0.1% acetonitrile-formic, a column of Poroshell 120 EC-C18 (100mm L x 2.1mm ID, 2.7μm) and the column temperature of 35℃. The analytes were quantitated by external standard method. Statistics indicated that this method whose RSD was 2.3~7.5%,had a good linear with R2>0.999 in their ranges of linearity, what’s more, the LODs of which were 0.2~2.0μg/kg and the LOQs were 0.6~6.0μg/kg along with a hige recovery rate ranged 75.1~89.3% from different sample matrixes (beef, chicken,pork liver) added 3 levels of concentration. In a word, it is suitable for rapid screening and quantitative determination of 19 antihistamines and their metabolitesin in animal derived food.

Key words: antihistamine, liquid chromatography-mass spectrometry (LC-MS), animal food, EMR-Lipid adsorbent

中图分类号:

O657.63

王京. 空间位阻净化-液相色谱-串联质谱技术测定动物源性食品中抗组胺类药物残留的方法研究[J]. 食品科学, 0, (): 0-0.

Jing WANG. Determination of antihistamine residues in animal derived foods by EMR-Lipid technology and LC-MS/MS[J]. FOOD SCIENCE, 0, (): 0-0.

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