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

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

Key words:  HPLC  tandem mass spectrometry  dispersive solid phase extraction  isotope dilution  patulin  health product

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WatersAtlantis-T3（3.0 mm×50 mm，5 μm）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5~500 μg·L^-1内线性关系良好，r²≥0.998 5；回收率为85.7%~93.4%，RSD（n=6）为3.2%~7.0%；定量限为5.0 μg·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。

Abstract:

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 r² ≥ 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.