GC-MS/MS 法测定尿液中甾体激素：固相衍生化法替代传统方法。
GC-MS/MS Determination of Steroid Hormones in Urine Using Solid-Phase Derivatization as an Alternative to Conventional Methods.
机构信息
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.
出版信息
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。
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