食品科学

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自制固相萃取柱-超高效液相色谱-串联质谱法同时测定果蔬中的8 种真菌毒素

王 蒙,姜 楠,韦迪哲,冯晓元*   

  1. 北京农业质量标准与检测技术研究中心,农业部农产品质量安全风险评估实验室(北京),北京 100097
  • 出版日期:2016-05-25 发布日期:2016-05-18

A Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Method for the Determination of 8 Mycotoxins in Fruits and Vegetables

WANG Meng, JIANG Nan, WEI Dizhe, FENG Xiaoyuan*   

  1. Risk Assessment Laboratory for Agro-Products (Beijing), Ministry of Agriculture, Beijing Research Center for Agricultural Standards and Testing, Beijing 100097, China
  • Online:2016-05-25 Published:2016-05-18

摘要:

建立基于自制固相萃取柱的样品净化-超高效液相色谱-串联质谱同时测定果蔬中8 种主要真菌毒素的方法,包括链格孢毒素、展青霉素、赭曲霉毒素A及橘青霉素。样品经80%乙腈溶液提取、离心后,通过自制固相萃取柱(HLB+MCX)排除杂质干扰,流出液经氮吹至近干后,直接用超高效液相色谱-串联质谱进行测定,基质外标法定量。在较宽的线性范围内,8 种毒素的线性相关系数(r2)均不小于0.99,定量限为1~5 μg/kg,在3 个不同添加水平下的加标回收率为76.0%~102.7%,相对标准偏差为0.8%~4.7%。该法灵敏度高,操作简单﹑快速,适用于苹果、樱桃和番茄等果蔬中痕量真菌毒素的测定。

关键词: 真菌毒素, 自制固相萃取柱, 超高效液相色谱-串联质谱, 果蔬

Abstract:

A novel method for the determination of 8 mycotoxins, including alternariol (AOH), alternariol monamethyl
ether (AME), tenuazonic acid (TeA), altenuene (ALT), tentoxin (TEN), patulin (PAT), ochratoxin A (OTA) and citrinin
(CIT) in fruits and vegetables was developed using a laboratory-prepared solid phase extraction (SPE) column coupled
with ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The sample was extracted with
80% acetonitrile solution, and cleaned up on the SPE column. The separation of the analytes was carried out on an Acquity
CORTECS UPLC C18 column (100 mm × 2.1 mm, 1.6 μm) using a mobile phase composed of a mixture of acetonitrile and
5 mmol/L ammonium acetate aqueous solution with gradient elution. The extract was determined by UPLC-MS/MS. Matrixmatched
calibration was used for the quantification. The proposed method showed a good linear correlation with correlation
coefficients all above 0.99. The recoveries for blank samples fortified at three levels ranged from 76.0% to 102.7% with
RSDs from 0.8% to 4.7%. The limits of detection (LODs) ranged from 1 to 5 μg/kg. The method possessed the advantages
of sensitivity, simplicity and fastness, and was successfully applied in the determination of low levels of mycotoxins residues
in apple, sweet cherry and tomato samples.

Key words: mycotoxins, laboratory-prepared solid phase extraction column, ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS), fruits and vegetables

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