Zhou Jian, Xu Jiao-Jiao, Cai Zeng-Xuan, Huang Bai-Fen, Jin Mi-Cong, Ren Yi-Ping
Lab of Physicochemical Research, Department of Physicochemical & Toxicology, Zhejiang Provincial Center for Disease Control and Prevention, Zhejiang 310051, China; Zhejiang Provincial Key Lab of Health Risk Appraisal for Trace Toxic Chemicals, Ningbo Municipal Center for Disease Control and Prevention, Ningbo 315010, China.
Lab of Physicochemical Research, Department of Physicochemical & Toxicology, Zhejiang Provincial Center for Disease Control and Prevention, Zhejiang 310051, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Nov 15;1068-1069:15-23. doi: 10.1016/j.jchromb.2017.10.001. Epub 2017 Oct 4.
Two analytical approaches, including ultra-high performance liquid chromatograph linked with photo-diode array/fluorescence detector, and ultra-high performance liquid chromatography-tandem mass spectrometry, have been proposed for simultaneous determination of five Alternaria toxins in cereals, which both based on QuEChERS strategy. After QuEChERS extraction and salting out, the collected supernatant was subjected to an extra dispersive liquid-liquid microextraction step prior to quantitative analysis. Response surface methodology based on central composite design was employed to optimize the micro-extraction conditions. During photo-diode array/fluorescence detector method validation, satisfactory analytical characteristics, in terms of selectivity, recovery (72.7%-109.1%), precision (inter-day RSDs <9.6%), sensitivity (limits of quantification ranged from 2.1μgkg to 120.0μgkg) and linearity (R all higher than 0.9984), were achieved. Mass spectrometry method was employed as a certified method for accuracy. The two methodologies were successfully applied to 71 samples including three different matrices and the quantitative results were compared. As the result of non-parametric test shown, the established two analytical approach exhibited comparable quantitative accuracy to each other.
已提出两种分析方法,包括超高效液相色谱仪与光电二极管阵列/荧光检测器联用以及超高效液相色谱-串联质谱法,用于同时测定谷物中的五种链格孢菌毒素,这两种方法均基于QuEChERS策略。经过QuEChERS萃取和盐析后,收集的上清液在进行定量分析之前要经过额外的分散液液微萃取步骤。采用基于中心复合设计的响应面法优化微萃取条件。在光电二极管阵列/荧光检测器方法验证过程中,在选择性、回收率(72.7%-109.1%)、精密度(日间相对标准偏差<9.6%)、灵敏度(定量限范围为2.1μg/kg至120.0μg/kg)和线性(相关系数均高于0.9984)方面获得了令人满意的分析特性。采用质谱法作为准确性的验证方法。这两种方法成功应用于包括三种不同基质的71个样品,并对定量结果进行了比较。非参数检验结果表明,所建立的两种分析方法相互之间具有相当的定量准确性。