College of Public Health, Capital Medical University, Beijing, 100069, People's Republic of China.
Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning, Beijing Center for Disease Prevention and Control, Beijing, 100013, People's Republic of China.
Environ Sci Pollut Res Int. 2019 Aug;26(22):22485-22493. doi: 10.1007/s11356-019-05483-6. Epub 2019 Jun 3.
A sensitive and reliable analytical method has been developed and validated for the determination of five Alternaria toxins, including tenuazonic acid (TeA), alternariol (AOH), alternariol monomethyl ether (AME), altenuene (ALT), and tentoxin (TEN), in drinking water using a one-step enrichment and clean-up strategy followed by ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). Drinking water samples were preprocessed using excess sodium sulfite to remove residual chlorine, and the pH was adjusted by formic acid. Analytes were concentrated and purified from the water samples using hydrophilic-lipophilic balanced (HLB) solid-phase extraction (SPE) cartridges. Chromatographic separation was performed on an Acquity HSS C column using 0.1 mM ammonium carbonate and methanol as the mobile phase. The average recoveries at three spiked levels (0.1, 0.5, and 1 ng/L for TeA, AOH, and ALT; 0.01, 0.05, and 0.1 ng/L for TEN and AME) were 76.1-106.5%, with an intra-day precision less than 15.5% and inter-day precision of 11.8-16.5%. The limits of detection (LODs) were 0.05 ng/L for TeA, AOH, and ALT and 0.005 ng/L for TEN and AME. The limits of quantification (LOQs) were 0.1 ng/L for TeA, AOH, and ALT and 0.01 ng/L for TEN and AME. The developed method was applied to monitor 289 drinking water samples collected in Beijing from 2015 to 2017, and TeA and TEN were found in 28 samples, with concentrations ranging from 0.16 to 2.7 ng/L and 0.21 to 2.2 ng/L, respectively.
建立并验证了一种灵敏、可靠的分析方法,用于采用一步式富集和净化策略,结合超高效液相色谱串联质谱(UPLC-MS/MS),测定饮用水中的五种交链孢霉毒素,包括交链孢酚(TeA)、交链孢酚单甲醚(AME)、Alternariol(AOH)、alternuene(ALT)和 tentoxin(TEN)。饮用水样品先用亚硫酸钠过量处理以去除余氯,再用甲酸调节 pH 值。用亲水-疏水平衡固相萃取(HLB-SPE)小柱从水样中浓缩和净化分析物。采用 Acquity HSS C 柱,以 0.1 mM 碳酸铵和甲醇为流动相进行色谱分离。在三个加标水平(TeA、AOH 和 ALT 的 0.1、0.5 和 1ng/L;TEN 和 AME 的 0.01、0.05 和 0.1ng/L)下,平均回收率为 76.1-106.5%,日内精密度小于 15.5%,日间精密度为 11.8-16.5%。检出限(LOD)为 TeA、AOH 和 ALT 的 0.05ng/L,TEN 和 AME 的 0.005ng/L。定量限(LOQ)为 TeA、AOH 和 ALT 的 0.1ng/L,TEN 和 AME 的 0.01ng/L。该方法应用于监测 2015 年至 2017 年期间在北京采集的 289 个饮用水样品,发现 28 个样品中存在 TeA 和 TEN,浓度范围分别为 0.16-2.7ng/L 和 0.21-2.2ng/L。