Pre-Concentration and Separation of Perphenazine Using Picric Acid Loaded α-Fe2O3 Nanoparticles: HPLC Syringe Filter as the Particles Support

Suspension of picric acid (PA) loaded iron oxide nanoparticles (PA-IONPs) was injected on the top of a 0.2 µm HPLC (high-performance liquid chromatography) syringe filter. The immobilized nanoparticles were used as SPE (solid phase extraction) sorbent for perphenazine separation and pre-concentration. By passing perphenazine solution through the filter, a molecular complex between perphenazine and PA was formed. Perphenazine/PA complex was eluted from the filter using dichloromethane as solvent. The perphenazine contents were determined at 254 nm. Effects of the parameters such as pH, the amount of PA-IONPs, as well as flow rate, volume, and type of eluting solvents, on the separation efficiency and pre-concentration of perphenazine were investigated. The calibration curve was linear in the range of 0.5-5 ng mL-1 (Y = 0.047X + 0.018; R2 = 0.9952) with limit of detection of 0.16 ng mL-1. The pre-concentration and enrichment factors were 8.33 and 1.88, respectively. This method was successfully applied to the determination of perphenazine residue in tap water.

将负载苦味酸（Picric Acid, PA）的氧化铁纳米颗粒（PA-IONPs）悬浮液注入0.2 μm高效液相色谱（High-Performance Liquid Chromatography, HPLC）针式过滤器的顶部。将该固定化纳米颗粒用作固相萃取（Solid Phase Extraction, SPE）吸附剂，用于奋乃静的分离与预富集。当奋乃静溶液流经该过滤器时，奋乃静与PA可形成分子复合物。以二氯甲烷作为洗脱溶剂，可将奋乃静/PA复合物从过滤器上洗脱下来。于254 nm波长处测定奋乃静的含量。考察了pH值、PA-IONPs投加量、流速、洗脱溶剂体积及洗脱溶剂种类等参数对奋乃静分离效率与预富集效果的影响。该方法的校准曲线在0.5~5 ng·mL⁻¹范围内呈良好线性关系（Y = 0.047X + 0.018；R² = 0.9952），检出限为0.16 ng·mL⁻¹。其预浓缩倍数与富集因子分别为8.33和1.88。本方法已成功应用于自来水中奋乃静残留量的测定。