Determination of Urinary Mycotoxin Biomarkers Using a Sensitive Online Solid Phase Extraction-UHPLC-MS/MS Method.
Determination of Urinary Mycotoxin Biomarkers Using a Sensitive Online Solid Phase Extraction-UHPLC-MS/MS Method.
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DOI：
10.3390/toxins13060418
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发表时间：
2021-06-11
期刊：
影响因子：
4.2
通讯作者：
Humpf HU
中科院分区：
文献类型：
--
作者：
Schmidt J;Cramer B;Turner PC;Stoltzfus RJ;Humphrey JH;Smith LE;Humpf HU
在评估人类暴露于真菌毒素的过程中，基于生物标记物的方法已被证明是重要的工具。低浓度水平、复杂的基质组成、结构多样化的分析物以及庞大的样本群是分析方法的主要挑战。为此，建立了在线固相萃取-超高效液相色谱-串联质谱仪(Online SPE-UHPLC-MS/MS)方法，可以灵敏、快速地分析人尿中11种相关真菌毒素和真菌毒素代谢物。分析物包括黄曲霉毒素M1、丙氨酸氨基转移酶、交链孢单甲醚、交链孢醇、桔霉素及其代谢物二氢桔青酮、伏马菌素B1、赭曲霉毒素A、玉米赤霉烯酮，以及α-和β-玉米赤霉烯醇(α-和β-ZEL)。除了ALT、AME和AOH使用基质校正外，通过稳定的同位素稀释法实现了可靠的定量。对方法性能的评价表明，方法检出限在Pg/mL尿液范围内较低，表观回收率令人满意，日内和日间重复性具有较高的准确度和精密度。在对津巴布韦尿样(n=50)的分析中，显示了新开发的方法的适用性。除了FB1在所有分析样本中都是可定量的外，还检测到了其他六种霉菌毒素生物标志物。与使用已建立的稀释和发射(DAS)方法分析相同样本集后获得的出现率相比，在应用在线固相萃取方法时观察到的阳性样本数量要高得多。由于提高了灵敏度，减少了样品处理的需要，并且花费了较少的时间，本文提出的在线固相萃取方法为真菌毒素暴露的人体生物监测提供了有价值的贡献。
In the course of assessing the human exposure to mycotoxins, biomarker-based approaches have proven to be important tools. Low concentration levels, complex matrix compositions, structurally diverse analytes, and the large size of sample cohorts are the main challenges of analytical procedures. For that reason, an online solid phase extraction-ultra high-performance liquid chromatography-tandem mass spectrometry (online SPE-UHPLC-MS/MS) method was developed, allowing for the sensitive, robust, and rapid analysis of 11 relevant mycotoxins and mycotoxin metabolites in human urine. The included spectrum of analytes comprises aflatoxin M1 (AFM1), altenuene (ALT), alternariol monomethyl ether (AME), alternariol (AOH), citrinin (CIT) and its metabolite dihydrocitrinone (DH-CIT), fumonisin B1 (FB1), ochratoxin A (OTA), and zearalenone (ZEN) as well as α- and β-zearalenol (α- and β-ZEL). Reliable quantitation was achieved by means of stable isotope dilution, except for ALT, AME and AOH using matrix calibrations. The evaluation of method performance displayed low limits of detection in the range of pg/mL urine, satisfactory apparent recovery rates as well as high accuracy and precision during intra- and interday repeatability. Within the analysis of Zimbabwean urine samples (n = 50), the applicability of the newly developed method was shown. In addition to FB1 being quantifiable in all analyzed samples, six other mycotoxin biomarkers were detected. Compared to the occurrence rates obtained after analyzing the same sample set using an established dilute and shoot (DaS) approach, a considerably higher number of positive samples was observed when applying the online SPE method. Owing to the increased sensitivity, less need of sample handling, and low time effort, the herein presented online SPE approach provides a valuable contribution to human biomonitoring of mycotoxin exposure.
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影响因子：
4.1
作者：
Campone, Luca;Piccinelli, Anna Lisa;Rastrelli, Luca
通讯作者：
Rastrelli, Luca
影响因子：
2
作者：
Rozentale, I;Bogdanova, E.;Bartkevics, V
通讯作者：
Bartkevics, V
影响因子：
4.3
作者：
Campone, Luca;Piccinelli, Anna Lisa;Rastrelli, Luca
通讯作者：
Rastrelli, Luca
DOI：
10.1016/j.ijheh.2019.06.010
发表时间：
2019-07-01
影响因子：
6
作者：
Martins, C.;Vidal, A.;Alvito, P.
通讯作者：
Alvito, P.
影响因子：
3
作者：
Bergmann, Dominik;Huebner, Florian;Humpf, Hans-Ulrich
通讯作者：
Humpf, Hans-Ulrich