高效液相色谱-串联质谱法测定乳和乳制品中19种苯并咪唑类药物及其代谢物残留量
高效液相色谱-串联质谱法测定乳和乳制品中19种苯并咪唑类药物及其代谢物残留量
目的建立高效液相色谱-串联质谱法测定乳和乳制品中19种苯并咪唑类药物及其代谢物残留量的方法。方法样品采用水-乙腈溶液提取, 氯化钠盐析, 饱和正己烷脱脂净化直接稀释后, 经Atlantis T3 (4.6 mm×100 mm, 3 μm)色谱柱分离, 以乙腈-0.1%甲酸溶液为流动相, 采用电喷雾离子源质谱, 在正离子扫描方式下以多反应监测(multiple response monitoring, MRM)模式检测, 外标法定量。结果19种苯并咪唑类药物及其代谢物在3个加标水平下的平均回收率为70.7%~110.0%, 相对标准偏差为2.3%~9.9%。在0.2~10 μg/L质量浓度范围内线性关系良好, 定量限为10~80 μg/kg。结论该方法操作简便, 灵敏度高, 抗干扰能力强, 回收率和重复性良好, 适用于乳和乳制品中苯并咪唑类药物及其代谢物的测定。
ObjectiveTo establish a method of determination of benzimidazoles and its metabolites residues in dairy and dairy products by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). MethodsThe sample was extracted with acetonitrile-water, then salted out by sodium chloride and degreased by hexane. The targeted compounds were separated with a Atlantis T3(4.6 mm×100 mm, 3 μm) with the mobile phases of acetonitrile and 0.1% formic acid and detected by electrospray ionization mass spectrometry in positive and multiple reaction monitoring (MRM) mode. The quantification was performed by the external standard method. ResultsThe recoveries at the 3 spiked levels were in the range of 70.7%?110.0% with the relative standard deviations in the range of 2.3%?9.9%. The calibration curves showed good linearity in the range of 0.2?10 μg/L. The limits of quantification were 10?80 μg/kg. ConclusionThis method is easy to operate, it has high sensitivity, strong anti-interference ability, good recovery and repeatability, which is suitable for the determination of benzimidazole drugs and their metabolites in milk and dairy products.
标题：高效液相色谱-串联质谱法测定乳和乳制品中19种苯并咪唑类药物及其代谢物残留量
英文标题：Determination of benzimidazoles and its metabolites residues in dairy and dairy products by high performance liquid chromatography-tandemmass spectrometry
作者：
陈思敏 广州海关技术中心；广东省动植物与食品进出口技术措施研究重点实验室
吴映璇 广州海关技术中心；广东省动植物与食品进出口技术措施研究重点实验室
邹游 广州海关技术中心；广东省动植物与食品进出口技术措施研究重点实验室
蓝草 广州海关技术中心；广东省动植物与食品进出口技术措施研究重点实验室
谢敏玲 广州海关技术中心；广东省动植物与食品进出口技术措施研究重点实验室
中文关键词:苯并咪唑类药物及其代谢物,高效液相色谱-串联质谱,乳制品,
英文关键词:benzimidazoles and its metabolites,high performance liquid chromatography-tandem mass,dairy products,
发表日期：2019-08-22
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