超高效液相色谱-四极杆-飞行时间质谱法快速检测发酵黑茶中黄曲霉毒素B_1

以直接提取稀释结合黄曲霉毒素免疫亲和柱净化的方法,利用超高效液相色谱-四极杆-飞行时间质谱(UPLC-Q-TOF-MS),建立了发酵黑茶中黄曲霉毒素B1(AFB1)的快速分析方法。样品采用甲醇-水溶液(7∶3,体积比)提取,以HSS T3色谱柱(100 mm×2.1 mm,1.8μm)进行色谱分离,通过正离子扫描,Full ms-dd-MS/MS模式进行分析。结果表明:33种发酵黑茶中的AFB1在一定范围内具有良好的线性关系,相关系数(r2)大于0.999,4种样品的加标回收率(n=4)为86.4%~98.0%,相对标准偏差(RSD)为0.3%~1.7%,检出限(LOD,S/N≥3)和定量下限(LOQ,S/N≥10)分别为0.06μg/kg和0.19μg/kg。结果显示33种样品中的AFB1含量均在合理范围内。该方法准确、快速、简单,适用于发酵黑茶中AFB1的检测。

Rapid Detection of Aflatoxin B1 in Fermented Dark Tea by Ultra Performance Liquid Chromatography-Quadrupole Time-of-Flight Mass Spectrometry

An ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometric (UPLC-Q-TOF-MS) method with purification of aflatoxin immunoaffinity column was established for the determination of aflatoxin B1 (AFB1) in fermented dark tea.The sample was extracted with methanol-water(7:3,by volume),and separated with an HSS T3 column(100 mm × 2.1 mm,1.8 μm),then scanned in positive ion scanning mode and analyzed in Full ms-dd-MS/MS mode.The results showed that there existed good linearities for aflatoxin B1 in 33 kinds of fermented dark tea in corresponding concentration range,with their correlation coefficients all greater than 0.999.The recoveries were in the range of 86.4％-98.0％ with the relative standard deviations (RSDs) of 0.3％-1.7％.The limits of detection(LODs,S/N≥3) and the limits of quantification (LOQs,S/N≥1O) were O.06 μg/kg and 0.19 μg/kg,respectively.This method was used to detect AFB1 in 33 tea samples collected from the local markets,and negative results were obtained.The results showed that the contents of AFB1 were within a reasonable range.This method was accurate,rapid and simple,and was suitable for the daily detection of AFB1.