| 在线固相萃取/高效液相色谱-四极杆/静电场轨道阱高分辨质谱检测饲料中的黄曲霉毒素 |
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| 中文摘要:建立了在线固相萃取/高效液相色谱-四极杆/静电场轨道阱高分辨质谱测定饲料中黄曲霉毒素B1（AFB1）、黄曲霉毒素B2（AFB2）、黄曲霉毒素G1（AFG1）及黄曲霉毒素G2（AFG2）的方法。采用IMMUNOPREP- ONLINE AFLATOXIN（Part Code:P900）柱为在线固相萃取柱，DiamonsilPlus C18（150 mm×4.6 mm,5 μm）柱为分析柱。样品中加入一定量的NaCl和乙腈-水（80∶20，体积比）溶解，超声提取后，用于后续进样。样品溶液注入在线固相萃取小柱中，通过阀切换技术和HPD共聚焦洗脱模式将保留在SPE柱上的靶标物转移到分析柱中继续进行分离分析，采用外标法定量，采用正离子全扫描模式进行分析。在优化的色谱-质谱条件下，该方法对4种黄曲霉毒素的线性范围为0.5~50.0 μg/L,检出限可达0.2 μg/kg，定量下限可达0.5 μg/kg。在0.5、1.0、5.0 μg/kg 3个加标水平下，饲料中4种黄曲霉毒素的回收率为94.6%~114.3%，相对标准偏差不大于8.3%。该方法分析时间短、自动化程度高、检测通量大、检测成本低，可作为饲料中AFB1、AFB2、AFG1、AFG2的快速检测方法。 |
| 中文关键词:黄曲霉毒素 在线固相萃取 高效液相色谱-四极杆/静电场轨道阱高分辨质谱 饲料 |
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| Determination of Aflatoxins in Feeds by High Performance Liquid Chromatography-Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry with Online Solid Phase Extraction |
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| Abstract:A high performance liquid chromatography-quadrupole/electrostatic field Orbitrap high resolution mass spectrometry（HPLC-Q/Orbitrap HRMS） was developed for the determination of aflatoxins in feeds.The IMMUNOPREP- ONLINE AFLATOXIN（Part Code:P900） was used as an online solid phase extraction column,and DiamonsilPlus C18（150 mm×4.6 mm,5 μm） as an analytical column.The feed samples were dissolved with a certain amount of NaCl and acetonitrile-water（80∶20）.After ultrasonic extraction,the supernatant was injected into an online solid phase extraction column,then the target was transferred to the analysis column by valve switching technique and HPD confocal elution mode for separation.The external standard method was used for quantitation.The analysis was performed by MS under Full scanning mode in positive mode.Under the optimal conditions,the calibration curves were linear in the range of 0.5-50.0 μg/L for four aflatoxin,the limits of detection and quantitation were 0.2 μg/kg and 0.5 μg/kg,respectively.The average recoveries at three spiked levels（0.5,1.0,5.0 μg/kg） were in the range of 94.6%-114.3% with relative standard deviations（RSDs） not more than 8.3%.With the advantages of rapidness,high automation,high-throughput detection and low cost,the proposed method could be used in the rapid detection on aflatoxins in feed samples. |
| Key Words:aflatoxins online solid phase extraction high performance liquid chromatography-quadrupole/electrostatic field Orbitrap mass spectrometry（HPLC-Q/Orbitrap MS） feed |
| 引用本文：刘飞，任安书，葛萍，丁年芳，娜仁·琪琪格.在线固相萃取/高效液相色谱-四极杆/静电场轨道阱高分辨质谱检测饲料中的黄曲霉毒素[J].分析测试学报,2018,37(6):696-701. |
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