分析测试学报2018，Vol.37Issue(6)：696-701,6.DOI:10.3969/j.issn.1004-4957.2018.06.009
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
Determination of Aflatoxins in Feeds by High Performance Liquid Chromatography-Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry with Online Solid Phase Extraction
刘飞 1任安书 1葛萍 1丁年芳 1娜仁·琪琪格1
作者信息
- 1. 南京华谱分析检测技术服务有限公司,江苏 南京 210001
- 折叠
摘要
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(R) ONLINE AFLATOXIN (Part Code: P900) was used as an online solid phase extraction column, and DiamonsilPlus C18(150 mm x4. 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.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Key words
aflatoxins/online solid phase extraction/high performance liquid chromatography-quadrupole/electrostatic field Orbitrap mass spectrometry(HPLC-Q/Orbitrap MS)/feed分类
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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):696-701,6.
