SiW11掺杂二氧化硅纳米纤维(SiW11/SiO2)的制备及对拟南芥叶中多胺的萃取分析

采用静电纺丝技术制备了SiW₁₁掺杂的二氧化硅纳米纤维(SiW₁₁/SiO₂)材料, 其中掺杂的SiW₁₁质量占纤维质量的7.83%, 制备的SiW₁₁/SiO₂材料尺寸均一, 在考察的pH范围内带负电, 与未掺杂SiW₁₁的二氧化硅纳米纤维相比, SiW₁₁/SiO₂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 dSPE)-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/mL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/mL. 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SiW₁₁/SiO₂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.

Preparation of SiW11 Incorporated SiO2 Nanofibers(SiW11/SiO2) and Its Application in the Analysis of Polyamines in Arabidopsis†

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/mL to 0.9 ng/mL, and the linear range was 10—1000 ng/mL and 20—1000 ng/mL 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.