Dmitrieva E V, Temerdashev A Z, Zorina M O, Feng Yu-Qi, Nesterenko P N
Kuban State University, Stavropolskaya st., 149, Krasnodar 350040, Russia.
Kuban State University, Stavropolskaya st., 149, Krasnodar 350040, Russia.
J Pharm Biomed Anal. 2022 May 30;214:114736. doi: 10.1016/j.jpba.2022.114736. Epub 2022 Mar 21.
A possibility of application of solid-phase analytical derivatization (SPAD) for the quantification of seven steroid hormones (testosterone, dihydrotestosterone, cortisone, cortisol, progesterone, 11α-hydroxyprogesterone, and estrone) in human urine was evaluated. To prepare urine samples for instrumental analysis, SPAD with hydroxylamine was applied after enzymatic hydrolysis of the sample. To achieve high recovery values, extraction and derivatization conditions were optimized. Cartridges packed with end-capped octadecylsilyl silica sorbent provided optimum extraction of target analytes, while the reaction with hydroxylamine in the cartridge was found as a simple and efficient way for the chemical derivatization of steroids. The obtained derivatives were detected by using reversed-phase ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry. The proposed procedure was validated and applied to the analysis of real urine samples to prove the applicability of the proposed method for the routine analysis.
评估了应用固相分析衍生化（SPAD）定量测定人尿中七种甾体激素（睾酮、二氢睾酮、可的松、皮质醇、孕酮、11α-羟基孕酮和雌酮）的可能性。为了制备用于仪器分析的尿液样本，在对样本进行酶水解后应用了与羟胺的SPAD。为了获得高回收率，对萃取和衍生化条件进行了优化。填充有封端十八烷基甲硅烷基硅胶吸附剂的小柱可实现目标分析物的最佳萃取，而在小柱中与羟胺的反应被发现是甾体化学衍生化的一种简单有效方法。使用反相超高效液相色谱-四极杆飞行时间质谱法检测得到的衍生物。对所提出的方法进行了验证，并应用于实际尿液样本的分析，以证明该方法在常规分析中的适用性。
