SiW_(11)掺杂二氧化硅纳米纤维(SiW_(11)/SiO_2)的制备及对拟南芥叶中多胺的萃取分析

Preparation of SiW_(11) Incorporated SiO_2 Nanofibers(SiW_(11)/SiO_2) and Its Application in the Analysis of Polyamines in Arabidopsis

采用静电纺丝技术制备了SiW_(11)掺杂的二氧化硅纳米纤维(SiW_(11)/SiO_2)材料,其中掺杂的SiW_(11)质量占纤维质量的7. 83%,制备的SiW_(11)/SiO_2材料尺寸均一,在考察的pH范围内带负电,与未掺杂SiW_(11)的二氧化硅纳米纤维相比,SiW_(11)/SiO_2材料表现出强阳离子交换作用,能有效萃取尸胺和腐胺.在最优条件下,建立了注射器分散固相萃取(In syringe d SPE)-超高效液相色谱-串联质谱联用(UHPLC-MS/MS)检测拟南芥样品中多胺的方法.结果表明,尸胺和腐胺分别在10～1000和20～1000 ng/m L浓度范围内具有良好的线性关系(R2≥0. 9950),检出限和定量限分别为0. 5～0. 9和1. 6～3. 0 ng/m L.将该方法应用于拟南芥样品中尸胺和腐胺的检测,加标回收率在87. 5%～111. 3%之间,相对标准偏差RSD<5. 0%.建立的SiW_(11)/SiO_2制备方法解决了多金属氧酸盐(POM)在修饰改性过程中存在的制备繁琐、固载量少的问题,拓宽了POM在分离领域中的应用.

SiW11 incorporated SiO2 nanofibers(SiW11/SiO2) was prepared by electrospinning technology. The mass of incorporated SiW11 accounted for 7. 83% of nanofibers. SiW11/SiO2 nanofiber possessed uniform structure with the diameter about 450 nm,and was negative charged in the pH range of 1. 0-11. 0. Compared with SiO2 nanofibers,the SiW11/SiO2 nanofiber exhibited stronger cation-exchange interactions to extract PUT and CAD. Under the optimized condition,an in-syringe dSPE-UHPLC-MS/MS method for rapid and selective detection of polyamines from plants was established. The limits of detection(LODs) for the target CAD and PUT ranged from 0. 5 ng/m L to 0. 9 ng/m L,and the linear range was 10-1000 ng/m L and 20-1000 ng/m L with determination coefficients(R2) higher than 0. 9950. The recoveries ranged from 87. 5% to 111. 3% with relative standard deviations(RSDs) of 1. 9%-7. 2%. The proposed method can be used to detect the trace CAD and PUT in Arabidopsis.