超高效液相色谱-串联质谱法检测牛奶中双氯芬酸钠残留  

Determination of diclofenac sodium in milk by ultra-high performance liquid chromatography-tandem mass spectrometry

作　　者：倪香艳 李建 孙志文[1] 怀文辉[1] 叶能胜[2] NiXiangyan;Li Jian;Sun Zhiwen;Huai Wenhui;Ye Nengsheng(Beijing Institute of Veterinary Drugs Control,Beijing 102200,China;Department of Chemistry,Capital Normal University,Beijing 100048,China)

机构地区：[1]北京市兽药监察所,北京102600 [2]首都师范大学化学系,北京100048

出　　处：《分析仪器》2018年第4期63-67,共5页Analytical Instrumentation

基　　金：北京市自然科学基金项目(2162008);北京市科学技术协会青年人才托举计划项目

摘　　要：建立了测定牛奶中双氯芬酸钠残留的超高效液相色谱-串联质谱法。试样经乙酸乙酯提取、正己烷去除脂类,采用C18反相色谱柱进行分离,乙腈-0.1%甲酸水(55+45)为流动相洗脱,电喷雾离子源正离子模式下多反应监测模式(MRM)检测,内标法定量。结果表明,双氯芬酸钠在0.05~5ng/mL浓度范围内线性良好,相关系数0.9996;该方法在牛奶中检测限(LOD,S/N=3)和定量限(LOQ,S/N=10)分别为0.02μg/kg和0.05μg/kg。3个浓度添加水平下,回收率97.6%~113.0%,日内变异系数0.5%~9.5%,日间变异系数1.8%~7.4%。方法快速、灵敏度高、重现性好,能快速准确测定牛奶中双氯芬酸钠残留。To determine the residue of diclofenac sodium in milk, an ultra-high performance liquid chromatography-tandem mass spectrometry method was established. The samples were extracted with ethyl acetate and hexane to remove the lipids. C18 reversed phase chromatographic column was used as the separation column, and acetonitrile-0.1 % formic acid water （55 ＋ 45） was used as the mobile phase. The scanning was monitored at multi-response monitoring mode （MRM） and the positive ions electrospray ion source mode was applied simultaneously,using the internal standard method for quantitative analysis. The results showed that diclofenac sodium was linear in the corresponding concentration range of 0.05 - 5 ng/mL,and the correlation coefficient was 0. 9996. The detection limit （LOD, S/N= 3） and quantitative limit （LOQ, S/N=10） of this method were 0.02 μg/kg and 0.05 μg/kg in milk, respectively. At the level of 3 spiked concentrations, the recoveries ranged from 97.6% to 113.0%, the variation coefficient of the intra-batch was within 0. 5 %-9.5 %, and the coefficient variation of the inter-batch was within 1.8 %- 7.4 %. The method is rapid, high sensitive and of good reproducibility, which is suitable for rapid determination of diclofenac sodium in milk.

关 键 词：超高效液相色谱-串联质谱法 双氯芬酸钠 牛奶 

分 类 号：O657.63[理学—分析化学] TS252.7[理学—化学]