CAS Key Laboratory of Separation Sciences for Analytical Chemistry, Department of Instrumentation & Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023, PR China; University of Chinese Academy of Sciences, Beijing 100039, PR China.
CAS Key Laboratory of Separation Sciences for Analytical Chemistry, Department of Instrumentation & Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023, PR China.
J Chromatogr A. 2020 May 10;1618:460894. doi: 10.1016/j.chroma.2020.460894. Epub 2020 Jan 15.
A green sample preparation method based on aqueous extraction followed by dispersive solid phase extraction (d-SPE) with in situ derivatization (ISD) was developed for the determination of aflatoxins (AFs) in traditional Chinese medicines (TCMs). AFs in TCMs were extracted by alkaline aqueous solution and converted to substituted coumaric acids. Then, mixed-mode anion exchange (MAX) sorbent was used to isolate and enrich the substituted coumaric acids. During the elution by acetonitrile/trifluoroacetic acid solution, AFs were reconstructed and in situ derivatized. Several parameters affecting the procedure were evaluated. The developed preparation method coupled with high performance liquid chromatography-fluorescence detection was successfully applied for AFs determination in TCMs. The limit of detection (LOD) reached 10 pg/mL for AFs. Good linearity was obtained in three orders of magnitude with correlation coefficients ranging from 0.9996 to 0.9999. The relative recoveries of the method were between 72.7% and 114.5% with intra- and inter-day relative standard deviations (RSDs) less than 9.5% and 10.1%, respectively. The method was successfully applied to determine AFs in 15 kinds of TCMs in China, with the results verified by IAC standard method.
建立了一种基于水相提取,随后采用分散固相萃取(d-SPE)结合原位衍生化(ISD)的绿色样品前处理方法,用于测定中药材中的黄曲霉毒素(AFs)。中药材中的 AFs 用碱性水溶液提取,并转化为取代香豆素酸。然后,使用混合模式阴离子交换(MAX)吸附剂分离和富集取代香豆素酸。在乙腈/三氟乙酸溶液洗脱过程中,AFs 被重建并原位衍生化。评价了影响该方法的几个参数。所建立的前处理方法与高效液相色谱-荧光检测联用,成功应用于中药材中 AFs 的测定。AFs 的检出限(LOD)达到 10 pg/mL。在三个数量级范围内,AFs 的线性关系良好,相关系数在 0.9996 到 0.9999 之间。该方法的相对回收率在 72.7%到 114.5%之间,日内和日间相对标准偏差(RSD)分别小于 9.5%和 10.1%。该方法成功应用于测定中国 15 种中药材中的 AFs,并通过 IAC 标准方法验证了结果。