Ran Congcong, Chen Dan, Ma Haiyan, Jiang Ye
Department of Pharmaceutical Analysis, School of Pharmacy, Hebei Medical University, 361 East Zhongshan Road, Shijiazhuang, Hebei, PR China.
Department of Pharmacy, Cangzhou Central Hospital, Cangzhou, Hebei, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Feb 15;1044-1045:120-126. doi: 10.1016/j.jchromb.2017.01.001. Epub 2017 Jan 3.
Graphene oxide (GO)-based dispersive solid phase extraction (D-SPE) method combined with multi-step preparation has been proposed for the evaluation of trace aflatoxins in proprietary Chinese medicines (PCM). After being extracted by methanol, the sample was purified based on multi-step preparation, including dehydration with MgSO/NaCl and cleanup with neutral alumina. Then GO was used as an adsorbent in D-SPE method for further preconcentration of aflatoxins prior to high performance liquid chromatography-fluorescence detection. The selected conditions were investigated. The Box-Behnken design (BBD) was used to optimize factors affecting adsorption procedure. Under the optimized conditions, good linear relationships had been achieved with the correlation coefficient (R) varying from 0.9904 to 0.9990. The LODs and LOQs were ranging from 0.020 to 0.041ng/mL and 0.061 to 0.125ng/mL, respectively. The results of the recoveries were 74.0-102.7% for the four aflatoxins, while the precisions from 1.8% to 7.2% were obtained, which indicated that the method was suitable for the analysis of aflatoxins in PCM.
本文提出了一种基于氧化石墨烯(GO)的分散固相萃取(D-SPE)方法,并结合多步制备过程,用于评估中成药(PCM)中的痕量黄曲霉毒素。样品经甲醇提取后,基于多步制备进行纯化,包括用MgSO/NaCl脱水和用中性氧化铝净化。然后,将GO用作D-SPE方法中的吸附剂,在高效液相色谱-荧光检测之前对黄曲霉毒素进行进一步预富集。对所选条件进行了研究。采用Box-Behnken设计(BBD)优化影响吸附过程的因素。在优化条件下,获得了良好的线性关系,相关系数(R)在0.9904至0.9990之间变化。检测限(LOD)和定量限(LOQ)分别为0.020至0.041ng/mL和0.061至0.125ng/mL。四种黄曲霉毒素的回收率为74.0-102.7%,精密度为1.8%至7.2%,表明该方法适用于中成药中黄曲霉毒素的分析。