Dong Maofeng, Si Wenshuai, Jiang Keqiu, Nie Dongxia, Wu Yongjiang, Zhao Zhihui, De Saeger Sarah, Han Zheng
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.
College of Pharmaceutical Sciences, Zhejiang University, 866 Yuhangtang Road, Hangzhou 310058, China.
J Chromatogr A. 2015 Dec 4;1423:177-82. doi: 10.1016/j.chroma.2015.10.068. Epub 2015 Oct 26.
A solid-phase extraction (SPE) procedure using multi-walled carbon nanotubes (MWCNTs) as sorbents coupled with ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was developed for simultaneous determination of four type A trichothecenes in maize, wheat and rice for the first time. Several key parameters including the composition of sample loading solutions, washing and elution solvents were thoroughly investigated to achieve optimal SPE recoveries and efficiency. Performance of the MWCNTs materials was significantly affected by pH, and after optimization, n-hexane and 5% methanol aqueous solution as the washing solutions and methanol containing 1% formic acid as the elution solvent presented an excellent purification efficiency for the four targets in the different matrices. The method was validated by determining the linearity (R(2)≥0.992), recovery (73.4-113.7%), precision (1.2-17.1%) and sensitivity (limit of quantification in the range of 0.02-0.10μg/kg), and was further applied for simultaneous determination of type A trichothecenes in 30 samples. Although low contamination levels of type A trichothecenes in wheat, maize and rice were observed revealing mitigated risks to consumers in Shanghai, China, the developed method has proven to be a valuable tool for type A trichothecenes monitoring in complex crop matrices.
首次开发了一种以多壁碳纳米管（MWCNTs）为吸附剂的固相萃取（SPE）方法，并结合超高效液相色谱-串联质谱（UHPLC-MS/MS）用于同时测定玉米、小麦和大米中的四种A型单端孢霉烯族毒素。对包括样品上样溶液组成、洗涤和洗脱溶剂在内的几个关键参数进行了深入研究，以实现最佳的SPE回收率和效率。MWCNTs材料的性能受pH值影响显著，优化后，正己烷和5%甲醇水溶液作为洗涤溶液，含1%甲酸的甲醇作为洗脱溶剂，对不同基质中的四种目标物具有优异的净化效率。通过测定线性（R(2)≥0.992）、回收率（73.4-113.7%）、精密度（1.2-17.1%）和灵敏度（定量限在0.02-0.10μg/kg范围内）对该方法进行了验证，并进一步应用于同时测定30个样品中的A型单端孢霉烯族毒素。尽管观察到中国上海的小麦、玉米和大米中A型单端孢霉烯族毒素的污染水平较低，对消费者的风险有所减轻，但所开发的方法已被证明是监测复杂作物基质中A型单端孢霉烯族毒素的有价值工具。
