Laboratory of Food Chemistry and Toxicology, Faculty of Pharmacy, University of Valencia, Av. Vicent Andres Estelles s/n, 46100 Burjassot, Spain.
Toxins (Basel). 2017 Oct 19;9(10):330. doi: 10.3390/toxins9100330.
The lower mycotoxin levels detected in urine make the development of sensitive and accurate analytical methods essential. Three extraction methods, namely salting-out liquid-liquid extraction (SALLE), miniQuEChERS (quick, easy, cheap, effective, rugged, and safe), and dispersive liquid-liquid microextraction (DLLME), were evaluated and compared based on analytical parameters for the quantitative LC-MS/MS measurement of 11 mycotoxins (AFB1, AFB2, AFG1, AFG2, OTA, ZEA, BEA, EN A, EN B, EN A1 and EN B1) in human urine. DLLME was selected as the most appropriate methodology, as it produced better validation results for recovery (79-113%), reproducibility (RSDs < 12%), and repeatability (RSDs < 15%) than miniQuEChERS (71-109%, RSDs <14% and <24%, respectively) and SALLE (70-108%, RSDs < 14% and < 24%, respectively). Moreover, the lowest detection (LODS) and quantitation limits (LOQS) were achieved with DLLME (LODs: 0.005-2 μg L, LOQs: 0.1-4 μg L). DLLME methodology was used for the analysis of 10 real urine samples from healthy volunteers showing the presence of ENs B, B1 and A1 at low concentrations.
尿液中检测到的真菌毒素水平越低，就越需要开发灵敏和准确的分析方法。本文基于 LC-MS/MS 定量分析方法，评估并比较了 3 种提取方法（盐析液-液萃取（SALLE）、miniQuEChERS（快速、简单、廉价、有效、耐用、安全）和分散液-液微萃取（DLLME）），以用于定量测定人尿中 11 种真菌毒素（AFB1、AFB2、AFG1、AFG2、OTA、ZEA、BEA、EN A、EN B、EN A1 和 EN B1）的分析参数。DLLME 被选为最合适的方法，因为与 miniQuEChERS（回收率为 71-109%，RSDs <14%和<24%）和 SALLE（回收率为 70-108%，RSDs <14%和<24%）相比，它在回收率（79-113%）、重现性（RSDs <12%）和重复性（RSDs <15%）方面产生了更好的验证结果。此外，DLLME 还实现了最低检测限（LODs）和定量限（LOQs）（LODs：0.005-2μg/L，LOQs：0.1-4μg/L）。该方法用于分析 10 份来自健康志愿者的真实尿液样本，结果表明存在低浓度的 ENs B、B1 和 A1。
