Jiang Keqiu, Huang Peng, Luan Lianjun, Fan Kai, Guo Wenbo, Zhao Zhihui, Wu Yongjiang, Han Zheng
College of Pharmaceutical Sciences, Zhejiang University, 866 Yuhangtang Road, Hangzhou 310058, China.
Institute for Agro-Food Standards and Testing Technology, Laboratory of Quality & Safety Risk Assessment for Agro-Products (Shanghai), Ministry of Agriculture, Shanghai Academy of Agricultural Sciences, Shanghai 201403, China.
J Chromatogr A. 2017 Jan 27;1482:1-10. doi: 10.1016/j.chroma.2016.12.058. Epub 2016 Dec 21.
For the first time, a reliable solid-phase extraction (SPE) procedure using iron (II, III) oxide (FeO)/multi-walled carbon nanotube (MWCNT) composite as sorbents was proposed for purification and enrichment of zearalenone (ZEA) and four type A trichothecenes (T-2 toxin (T-2), HT-2 toxin (HT-2), neosolaniol (NEO) and diacetoxyscirpenol (DAS)) in Salviae miltiorrhiza Radix et Rhizoma (Danshen). The FeO/MWCNT composite was synthesized by assembling FeO with MWCNT by sonication through an "aggregation wrap" mechanism and several key parameters affecting the performance of SPE procedure such as the composition of sample loading solutions, washing and elution solvents were thoroughly investigated. After optimization, 2% acetonitrile aqueous solution as the loading solution, 5% methanol aqueous solution as the washing solution and acetone containing 0.5% formic acid as the elution solvent presented an excellent purification efficiency for the five targets in Danshen. Under the optimal sample pretreatment conditions followed by analysis with ultra-high performance liquid chromatography-tandem mass spectrometry, satisfactory linearity (R≥0.991), high sensitivity (limit of quantification in the range of 1.20-4.80μgkg), good recovery (73.7-91.9%) and acceptable precision (RSD, 2.1-13.3%) were obtained. The applicability of the validated method was further verified in real Salviae miltiorrhiza Radix et Rhizoma samples.
首次提出了一种可靠的固相萃取(SPE)方法,该方法使用氧化铁(II, III)(FeO)/多壁碳纳米管(MWCNT)复合材料作为吸附剂,用于丹参中玉米赤霉烯酮(ZEA)和四种A型单端孢霉烯族毒素(T-2毒素(T-2)、HT-2毒素(HT-2)、新茄病镰刀菌烯醇(NEO)和二醋酸藨草镰刀菌烯醇(DAS))的净化和富集。通过超声处理,利用“聚集包裹”机制将FeO与MWCNT组装合成了FeO/MWCNT复合材料,并深入研究了影响SPE方法性能的几个关键参数,如样品加载溶液的组成、洗涤和洗脱溶剂。优化后,2%乙腈水溶液作为加载溶液,5%甲醇水溶液作为洗涤溶液,含0.5%甲酸的丙酮作为洗脱溶剂,对丹参中的五种目标物具有优异的净化效率。在最佳样品预处理条件下,采用超高效液相色谱-串联质谱法进行分析,获得了令人满意的线性关系(R≥0.991)、高灵敏度(定量限在1.20-4.80μg/kg范围内)、良好的回收率(73.7-91.9%)和可接受的精密度(相对标准偏差,2.1-13.3%)。在实际丹参样品中进一步验证了该验证方法的适用性。