Zhang Wenmin, Lin Mingxia, Tong Ping, Lu Qiaomei, Zhang Lan
Ministry of Education Key Laboratory of Analysis and Detection for Food Safety, Fujian Provincial Key Laboratory of Analysis and Detection Technology for Food Safety, College of Chemistry, Fuzhou University, Fuzhou, Fujian 350116, China.
Ministry of Education Key Laboratory of Analysis and Detection for Food Safety, Fujian Provincial Key Laboratory of Analysis and Detection Technology for Food Safety, College of Chemistry, Fuzhou University, Fuzhou, Fujian 350116, China; Testing Center, The Sport Science Research Center, Fuzhou University, Fuzhou, Fujian 350002, China.
J Chromatogr A. 2016 Apr 22;1443:54-61. doi: 10.1016/j.chroma.2016.03.055. Epub 2016 Mar 24.
A simple, rapid and sensitive method for determination of trace levels of domoic acid (DA) in seawater was developed, based on a magnetic solid-phase extraction (MSPE) followed by high-performance liquid chromatography with tandem mass spectrometry (HPLC-MS/MS). Five kinds of ferrite magnetic nanospheres (MFe2O4; M=Fe, Co, Ni, Cu and Zn) were prepared and first used as sorbents for MSPE of DA and removal of salt interference. Under the same extraction and elution conditions, CuFe2O4 magnetic nanospheres provided the best pretreatment performance, which were then characterized in detail. After further optimization of conditions, the developed method showed good linearity (r(2)=0.9991) with the range of 5-1000 pg mL(-1), low limit of detection (2.5 pg mL(-1); S/N=3:1), low limit of quantification (5.0 pg mL(-1); S/N=10:1), and good recoveries (86.0-98.1%) with acceptable repeatability (RSD ≤ 6.5%; n=3) in seawater samples. The results demonstrated that the ferrite magnetic nanospheres are promising sorbents for efficient extraction of highly polar analytes from high ionic strength solutions.
基于磁固相萃取(MSPE)结合高效液相色谱-串联质谱(HPLC-MS/MS),开发了一种简单、快速且灵敏的测定海水中痕量软骨藻酸(DA)的方法。制备了五种铁氧体磁性纳米球(MFe2O4;M = Fe、Co、Ni、Cu和Zn),并首次用作DA的MSPE吸附剂及去除盐干扰。在相同的萃取和洗脱条件下,CuFe2O4磁性纳米球表现出最佳的预处理性能,并对其进行了详细表征。进一步优化条件后,所开发的方法在5 - 1000 pg mL(-1)范围内具有良好的线性(r(2)=0.9991)、低检测限(2.5 pg mL(-1);S/N = 3:1)、低定量限(5.0 pg mL(-1);S/N = 10:1),并且在海水样品中具有良好的回收率(86.0 - 98.1%)和可接受的重复性(RSD≤6.5%;n = 3)。结果表明,铁氧体磁性纳米球是从高离子强度溶液中高效萃取高极性分析物的有前景的吸附剂。