Analytical Chemistry Department, Kuban State University, Stavropolskaya st., 149, 350040 Krasnodar, Russia.
Physical Chemistry Department, M.V. Lomonosov Moscow State University, Leninskie Gory, 1, 119991 Moscow, Russia.
Molecules. 2022 Sep 7;27(18):5796. doi: 10.3390/molecules27185796.
Solid-phase analytical derivatization (SPAD) is a promising hybrid sample preparation technique combining the clean-up and preconcentration of the sample in a single step. In this work, a novel SPAD method based on the preparation of trimethylsilyl (TMS) derivatives of steroid hormones (testosterone, estrone, DHT, estriol, estradiol, and progesterone) in Phenomenex Strata C18-E (100 mg, 1 mL) cartridges has been developed and applied for their GC-MS/MS determination in human urine samples. The proposed procedure allows the detection and quantification of steroids with limits of 1.0-2.5 and 2.5-5 ng/mL, respectively. These characteristics are comparable with those obtained with a conventional liquid-liquid extraction, while the recovery of analytes in the proposed SPAD procedure is higher. The major advantages of SPAD are a short derivatization time, high efficiency, and the possibility to automatize the procedure. However, its cost-effectiveness in routine practice is still questionable.
固相分析衍生化 (SPAD) 是一种很有前途的混合样品制备技术，可在单个步骤中同时完成样品的净化和浓缩。在这项工作中，开发了一种基于制备类固醇激素（睾酮、雌酮、DHT、雌三醇、雌二醇和孕酮）的三甲硅烷基（TMS）衍生物的新型 SPAD 方法，并将其应用于人类尿液样品中类固醇的 GC-MS/MS 测定。该方法可检测和定量分别为 1.0-2.5 和 2.5-5 ng/mL 的类固醇。这些特征与传统液-液萃取获得的特征相当，而在提议的 SPAD 程序中分析物的回收率更高。SPAD 的主要优点是衍生化时间短、效率高，并且有可能实现自动化。然而，它在常规实践中的成本效益仍值得商榷。
