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

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。

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

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.