Beijing Research Center for Agricultural Standards and Testing, No. 9 Middle Road of Shuguanghuayuan, Haidian District, Beijing 100097, China.
Risk Assessment Laboratory for Agro-Products, Ministry of Agriculture, No. 9 Middle Road of Shuguanghuayuan, Haidian District, Beijing 100097, China.
Toxins (Basel). 2018 Oct 10;10(10):409. doi: 10.3390/toxins10100409.
One-step solid-phase extraction (SPE) using a multiwalled carbon nanotube (MWCNT) for simultaneous analysis of 21 mycotoxins, including nine trichothecenes, zearalenone (ZEN) and its derivatives, four aflatoxins, and two ochratoxins, in corn and wheat was developed. Several key parameters affecting the performance of the one-step SPE procedure-types of MWCNT, combinations with five sorbents (octadecylsilyl (C), hydrophilic⁻lipophilic balance (HLB), mixed-mode cationic exchange (MCX), silica gel, and amino-propyl (NH₂)), and filling amounts of the MWCNTs-were thoroughly investigated. The combination of 20 mg carboxylic MWCNT and 200 mg C was proven to be the most effective, allowing the quantification of all analyzed mycotoxins in corn and wheat. Under the optimized cleanup procedure prior to ultraperformance liquid chromatography⁻tandem mass spectrometry (UPLC⁻MS/MS) analysis, the method was validated by analyzing samples spiked at the limit of quantification (LOQ), two-times LOQ, and 10-times LOQ. Satisfactory linearity (² ≥ 0.9910), high sensitivity (LOQ in different ranges of 0.5⁻25 μg L), good recovery (75.6⁻110.3%), and acceptable precision (relative standard deviation (RSD), 0.3⁻10.7%) were obtained. The applicability of the method was further confirmed using raw samples of corn and wheat. In conclusion, the established method was rapid, simple and reliable for simultaneous analysis of 21 mycotoxins in corn and wheat.
采用多壁碳纳米管(MWCNT)一步固相萃取(SPE),同时分析玉米和小麦中的 21 种真菌毒素,包括 9 种单端孢霉烯族毒素、玉米赤霉烯酮(ZEN)及其衍生物、4 种黄曲霉毒素和 2 种赭曲霉毒素。研究了影响一步 SPE 程序性能的几个关键参数,包括 MWCNT 的类型、与 5 种吸附剂(十八烷基硅烷(C)、亲水-亲脂平衡(HLB)、混合模式阳离子交换(MCX)、硅胶和氨基丙基(NH₂))的组合以及 MWCNT 的填充量。结果表明,20mg 羧酸 MWCNT 和 200mg C 的组合效果最佳,可定量分析玉米和小麦中的所有分析真菌毒素。在优化的超高效液相色谱-串联质谱(UPLC-MS/MS)分析前净化程序下,采用该方法对限量(LOQ)、2 倍 LOQ 和 10 倍 LOQ 进行加标分析,验证了方法的有效性。该方法具有良好的线性(²≥0.9910)、高灵敏度(LOQ 在不同范围内为 0.5-25μg/L)、良好的回收率(75.6%-110.3%)和可接受的精密度(相对标准偏差(RSD)为 0.3%-10.7%)。该方法还通过玉米和小麦的原始样品进一步验证了其适用性。总之,该方法快速、简单、可靠,可用于同时分析玉米和小麦中的 21 种真菌毒素。