School of Pharmaceutical Sciences, Zhengzhou University, Zhengzhou 450001, China; Key Laboratory of Targeting Therapy and Diagnosis for Critical Diseases of Henan Province, Zhengzhou 450001, China.
School of Pharmaceutical Sciences, Zhengzhou University, Zhengzhou 450001, China.
Food Chem. 2023 Jul 30;415:135788. doi: 10.1016/j.foodchem.2023.135788. Epub 2023 Feb 24.
This study presents an in-pipette-tip kapok fiber-supported liquid extraction/in-situ derivatization (in-pipette-tip KF-SLE-ISD) method for simultaneous enrichment and derivatization of furfurals. Briefly, 3 mg of natural kapok fiber, which was loaded in an assembled pipette-tip, was used to support 12.5 μL of extractant (ethyl acetate/toluene, 75:25, v/v) containing 10 mM 2,4-dinitrophenylhydrazine. The in-pipette-tip KF-SLE-ISD procedure was conveniently conducted by aspirating/releasing 1 mL of sample solution 10 cycles, allowing simultaneous extraction and derivatization of furfurals. Then, 100 μL of acetonitrile was aspirated/released 5 cycles for elution, 10 μL of which was directly analyzed by high-performance liquid chromatography. The limits of quantitation were in ranges of 0.10-0.45 μg/mL. The method showed satisfied linearity (R > 0.99), precision (RSD < 8.53%) and relative recovery (90.34-114.71%), which was successfully applied to determine furfurals in various samples (e.g., honeys, juices and glucose injections). The proposed method has the merits of effectiveness, simplicity, low cost, wide availability and ease of automation.
本研究提出了一种在管内尖端剑麻纤维支撑的液相萃取/原位衍生（in-pipette-tip KF-SLE-ISD）方法，用于糠醛的同时富集和衍生化。简要地说，将 3mg 的天然剑麻纤维装入组装好的微量进样管中，用于支撑 12.5μL 的萃取剂（乙酸乙酯/甲苯，75:25，v/v），其中含有 10mM 的 2,4-二硝基苯肼。通过 10 个循环的吸液/释放 1mL 样品溶液方便地进行管内尖端 KF-SLE-ISD 程序，允许糠醛的同时萃取和衍生化。然后，吸液/释放 5 个循环以洗脱 100μL 的乙腈，直接取 10μL 通过高效液相色谱进行分析。定量限在 0.10-0.45μg/mL 的范围内。该方法表现出令人满意的线性（R＞0.99）、精密度（RSD＜8.53%）和相对回收率（90.34-114.71%），成功地应用于各种样品（例如，蜂蜜、果汁和葡萄糖注射液）中糠醛的测定。该方法具有有效、简单、成本低、广泛可用性和易于自动化的优点。
