食品科学 ›› 2023, Vol. 44 ›› Issue (12): 368-375.doi: 10.7506/spkx1002-6630-20220715-174

• 安全检测 • 上一篇    下一篇

超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法同时筛查和测定番茄中11 种真菌毒素

王昌钊,李子豪,张亚莉,林芳,李建华,邹阳,杨玥   

  1. (1.西安海关技术中心,陕西 西安 710068;2.陕西省食品药品检验研究院,陕西 西安 710065;3.陕西中检检测技术有限公司,陕西 西安 710068)
  • 出版日期:2023-06-25 发布日期:2023-06-30
  • 基金资助:
    陕西省创新能力支撑计划项目(2019PT-22)

Simultaneous Screening and Determination of Eleven Mycotoxins in Tomato by Ultra-high Performance Liquid Chromatography-Quadrupole/Orbitrap High-Resolution Mass Spectrometry

WANG Changzhao, LI Zihao, ZHANG Yali, LIN Fang, LI Jianhua, ZOU Yang, YANG Yue   

  1. (1. Xi’an Customs Technology Center, Xi’an 710068, China; 2. Shaanxi Institute for Food and Drug Control, Xi’an 710065, China;3. Shaanxi Zhongjian Test Technology Co. Ltd., Xi’an 710068, China)
  • Online:2023-06-25 Published:2023-06-30

摘要: 建立使用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法同时对番茄中11 种真菌毒素筛查和定量的方法。样品经1%甲酸-乙腈提取后,用QuEChERS提取包盐析,并经分散型固相萃取净化管净化,采用ACQUITY UPLC BEH shield RP18(100 mm×2.1 mm,1.7 μm)色谱柱分离,在电喷雾离子源正负离子同时扫描及平行反应监测模式下,使用内标法和外标法定量,同时利用二级碎片离子建立筛查数据库,实现11 种真菌毒素的快速筛查。结果表明,11 种真菌毒素在0.25~100.0 mg/L范围内线性良好,相关系数(R2)均大于0.991,检出限为0.1~10.0 mg/kg,定量限为0.3~30.0 mg/kg,在低(1 倍定量限)、中(2 倍定量限)、高(10 倍定量限)3 个水平进行加标回收率实验,其平均回收率为78.5%~108.7%,相对标准偏差为1.0%~9.3%(n=6)。该方法操作简单、灵敏度高、结果准确,适合于番茄中11 种真菌毒素的快速筛查和准确定量。

关键词: 超高效液相色谱-四极杆/静电场轨道阱高分辨质谱;番茄;QuEChERS;真菌毒素

Abstract: A method was developed for the simultaneous screening and determination of eleven mycotoxins in tomato by ultra-high performance liquid chromatography-quadrepole/orbitrap high-resolution mass spectrometry (UPLC-Q/Orbitrap HRMS). Samples were extracted with a mixture of 1% formic acid solution and acetonitrile (99:1, V/V), salted out using a QuEChERS (quick, easy, cheap, effective, rugged and safe) extraction packet, and purified by dispersive solid phase extraction (dSPE). The target compounds were separated on an ACQUITY UPLC BEH shield RP18 column (100 mm × 2.1 mm, 1.7 μm), detected using an electrospray ionization source under positive and negative ion scanning with parallel reaction monitoring. A tandem mass spectral library for rapid screening of the eleven mycotoxins was built based on characteristic fragment ions. The results showed a good linear relationship in the concentration range of 0.25–100.0 mg/L, with correlation coefficients (R2) more than 0.991. The limit of detection (LOD) ranged from 0.1 to 10.0 μg/kg, and the limit of quantification (LOQ) ranged from 0.3 to 30.0 μg/kg. Average recoveries at three spiked levels, LOQ, 2 × LOQ, and 10 × LOQ, were in the range of 78.5%–108.7% with relative standard deviations from 1.0% to 9.3% (n = 6). This method proved to be simple, sensitive, accurate, and suitable for rapid screening and accurate quantification of the eleven mycotoxins in tomato.

Key words: ultra-high performance liquid chromatography-quadrupole/orbitrap high-resolution mass spectrometry; tomato; QuEChERS; mycotoxins

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