分散固相萃取-同位素稀释-HPLC-MS/MS测定保健食品中的展青霉素  

Determination of Patulin in Health Products by HPLC-MS/MS with Isotope Dilution and Dispersive Solid Phase Extraction

作　　者：林伟杰 励炯[1] 贾彦博[1] 王红青 孙岚 LIN Weijie;LI Jiong;JIA Yanbo;WANG Hongqing;SUN Lan(Hangzhou Institute for Food and Drug Control,Hangzhou 310017,China)

机构地区：[1]杭州市食品药品检验研究院

出　　处：《中国现代应用药学》2019年第19期2426-2430,共5页Chinese Journal of Modern Applied Pharmacy

基　　金：浙江省食品药品监管系统科技计划项目(SP2018004)

摘　　要：目的建立保健食品中展青霉素的分散固相萃取净化-同位素稀释高效液相色谱-串联质谱检测方法。方法样品经酶解后,经乙腈提取,加无水硫酸镁、C18-N以及NH2-PSA组成的净化剂后旋涡振荡,对样品进行净化,以Waters Atlantis-T3(3.0mm×50mm,5μm)色谱柱分离,流动相为乙腈-水(20∶80),负离子模式电喷雾电离,配合多反应离子扫描(MRM)定性定量分析目标化合物。考察净化剂中无水硫酸镁、C18-N、NH2-PSA的用量对加标回收率的影响,优化主要的影响因素和实验条件。结果展青霉素浓度在5~500μg·L^-1内线性关系良好,r^2≥0.998 5;回收率为85.7%~93.4%,RSD(n=6)为3.2%~7.0%;定量限为5.0μg·kg^-1。结论该方法适用于保健食品中展青霉素残留的检测分析。OBJECTIVE To develop an HPLC-MS/MS with isotope dilution and dispersive solid phase extraction method to determine patulin in health products. METHODS Enzymolysis samples were extracted with acetonitrile, and then purified by a mixture of anhydrous sodium sulfate, C18-N and NH2-PSA. The analysis was performed by a HPLC-MS/MS system with Waters Atlantis-T3(3.0 mm×50 mm, 5 μm) column. The mobile phase consisted of acetonitrile and water(20∶80), and multiple reaction monitoring(MRM) mode with negative electrospray ionization was used. The effect of the dosages of anhydrous magnesium sulfate, C18-N and NH2-PSA in cleaning-up agent was studied. The main influence factors and analytical conditions were modified. RESULTS The linear calibration curve was obtained with r^2≥0.998 5. The recoveries were ranged from 85.7% to 93.4%. RSD(n=6) ranged from 3.2% to 7.0%. The LOQ was 5.0 μg·kg^-1. CONCLUSION It is suitable for the determination of patulin in health products.

关 键 词：高效液相色谱法 串联质谱 分散固相萃取 同位素稀释 展青霉素 保健食品 

分 类 号：R917.101[医药卫生—药物分析学]