Pharmaceutical Analysis Department, School of Pharmacy, Fudan University, Shanghai 201203, Pudong, China.
Department of Dermatology, Ruijin Hospital, School of Medicine, Shanghai Jiaotong University, Shanghai 200025, Pudong, China.
J Pharm Biomed Anal. 2021 Jul 15;201:114101. doi: 10.1016/j.jpba.2021.114101. Epub 2021 May 1.
Lysophosphatidylcholine (LPC) was commonly known as a class of significant differential metabolites of high relevance with many diseases including psoriasis, of which the accurate determination is of great importance to diagnosis or prediction to many diseases. However, it is challenging and complicated because of the enormous biological sample complexity and impurities interference. In this study, we synthesized a magnetic nanocomposite MG@PD@TiO and took advantage of the interactions of Lewis acid-base between the phosphate groups in LPCs and Ti ions on MG@PD@TiO nanomaterials for selective separation and enrichment of LPCs from complex biological matrix. The solid-phase extraction sample pretreatment process by means of MG@PD@TiO nanomaterials coupled with LC-MS/MS method was then applied to actual determination of six typical LPCs (LPC 10:0, 14:0, 16:0, 18:0, 18:1, 22:0) in human plasma. The extraction conditions were scientifically optimized by single-factor test (adsorbent amount, adsorption and desorption time, elution solvent type, eluant volume). Under the optimal conditions, the detection limits (LOD, S/N = 3) and quantification limits (LOQ, S/N = 10) were 1 and 5 ng/mL for LPC 10:0 and LPC 14:0, 0.02 and 0.1 ng/mL for LPC 16:0 and LPC 18:1, 0.05 and 0.2 ng/mL LPC 18:0 and LPC 22:0, respectively. The intra- and inter-day precisions were 3.82-12.60 % (n = 6) and 3.29-13.50 % (n = 6) respectively, the recoveries were in the range of 91.92-113.69 % and the stability of the analytes in the matrix performed well with RSDs≤15.51 %. Finally, the developed method was successfully applied to the accurate determination of six LPCs biomarkers of plasma in patients with psoriasis (n = 10) and control groups (n = 10).
溶血磷脂酰胆碱（LPC）是一类具有重要差异的代谢物，与包括银屑病在内的许多疾病高度相关，其准确测定对许多疾病的诊断或预测具有重要意义。然而，由于生物样本的复杂性和杂质的干扰，其测定具有挑战性和复杂性。在本研究中，我们合成了磁性纳米复合材料 MG@PD@TiO，并利用 LPC 中磷酸基团与 MG@PD@TiO 纳米材料上 Ti 离子之间的路易斯酸碱相互作用，从复杂的生物基质中选择性分离和富集 LPC。然后，通过 LC-MS/MS 方法，采用 MG@PD@TiO 纳米材料的固相萃取样品预处理过程，应用于实际测定人血浆中的六种典型 LPC（LPC 10:0、14:0、16:0、18:0、18:1、22:0）。通过单因素试验（吸附剂用量、吸附和解吸时间、洗脱溶剂类型、洗脱体积）对提取条件进行了科学优化。在最佳条件下，LPC 10:0 和 LPC 14:0 的检测限（LOD，S/N = 3）和定量限（LOQ，S/N = 10）分别为 1 和 5 ng/mL，LPC 16:0 和 LPC 18:1 分别为 0.02 和 0.1 ng/mL，LPC 18:0 和 LPC 22:0 分别为 0.05 和 0.2 ng/mL。日内和日间精密度分别为 3.82-12.60%（n = 6）和 3.29-13.50%（n = 6），回收率在 91.92-113.69%之间，分析物在基质中的稳定性良好，RSDs≤15.51%。最后，该方法成功应用于银屑病患者（n = 10）和对照组（n = 10）血浆中六种 LPC 生物标志物的准确测定。
