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

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

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(r^2)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 novel method for the determination of 8 mycotoxins, including alternariol（AOH）, alternariol monamethyl ether（AME）, tenuazonic acid（Te A）, 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 C_（18） 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.