Department of Analytical Chemistry and Pollutants, Shahid Beheshti University, G. C., Evin, 1983969411, Tehran, Iran.
Anal Bioanal Chem. 2021 Dec;413(30):7609-7623. doi: 10.1007/s00216-021-03725-6. Epub 2021 Oct 19.
Therapeutic peptides have an important effect on physiological function and human health, so it is momentous to quantify and detect low levels of these biomolecules in biological samples for treatment and diagnostic purposes. In the present study, an efficient magnetic solid-phase extraction (MSPE) method was developed based on stearic acid-functionalized magnetic hydroxyapatite nanocomposite (MHAP/SA) as a novel and cost-effective adsorbent for extraction of five hypothalamic-related peptides (goserelin, octreotide, triptorelin, somatostatin, and cetrorelix) from biological samples. To characterize the morphology and physicochemical properties of MHAP/SA, Fourier transform infrared spectroscopy (FT-IR), energy-dispersive X-ray spectroscopy (EDS), field emission scanning microscopy (FE-SEM), CHNS elemental analysis, Brunauer-Emmett-Teller (BET), and vibrating sample magnetometry (VSM) were applied. Under optimum conditions, the proposed method (MSPE-HPLC-UV) represented favorable linearity with R ≥ 0.9987, suitable intra- and inter-day precisions (RSD ≤ 6.9% and RSD ≤ 8.1%, respectively, n = 3), and limits of detection and quantification in the range of 0.75-1.12 ng mL and 2.50-3.75 ng mL, respectively. Eventually, the proposed method was used for the extraction and quantification of target therapeutic peptides in plasma and urine samples, and satisfactory relative recoveries were achieved in the range of 90.6-110.3%.
治疗性肽对生理功能和人类健康有重要影响，因此定量和检测生物样本中这些生物分子的低水平对于治疗和诊断目的至关重要。在本研究中，基于硬脂酸功能化磁性羟基磷灰石纳米复合材料 (MHAP/SA) 开发了一种高效的磁固相萃取 (MSPE) 方法，作为一种新型且经济高效的吸附剂，用于从生物样本中提取五种下丘脑相关肽 (戈舍瑞林、奥曲肽、曲普瑞林、生长抑素和西曲瑞克)。为了表征 MHAP/SA 的形貌和物理化学性质，应用了傅里叶变换红外光谱 (FT-IR)、能谱 (EDS)、场发射扫描电子显微镜 (FE-SEM)、CHNS 元素分析、BET 和振动样品磁强计 (VSM)。在最佳条件下，所提出的方法 (MSPE-HPLC-UV) 表现出良好的线性关系，R 值≥0.9987，具有合适的日内和日间精密度 (RSD≤6.9%和 RSD≤8.1%，n=3)，检测限和定量限在 0.75-1.12 ng mL 和 2.50-3.75 ng mL 范围内。最终，该方法用于血浆和尿液样本中目标治疗性肽的提取和定量，相对回收率在 90.6-110.3%范围内。
