| 引用本文: | 林伟杰,励炯,贾彦博,王红青,孙岚.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[J].中国现代应用药学,2019,36(19):2426-2430. |
| LIN Weijie,LI Jiong,JIA Yanbo,WANG Hongqing,SUN Lan.Determination of Patulin in Health Products by HPLC-MS/MS with Isotope Dilution and Dispersive Solid Phase Extraction[J].Chin J Mod Appl Pharm(中国现代应用药学),2019,36(19):2426-2430. |
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| 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。 |
| 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 |
| DOI：10.13748/j.cnki.issn1007-7693.2019.19.012 |
| 分类号:R917.101 |
| 基金项目:浙江省食品药品监管系统科技计划项目（SP2018004） |
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| Determination of Patulin in Health Products by HPLC-MS/MS with Isotope Dilution and Dispersive Solid Phase Extraction |
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LIN Weijie, LI Jiong, JIA Yanbo, WANG Hongqing, SUN Lan
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Hangzhou Institute for Food and Drug Control, Hangzhou 310017, China
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| 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. |
| Key words: HPLC tandem mass spectrometry dispersive solid phase extraction isotope dilution patulin health product |
