Solid-phase analytical derivatization as a tool for the quantification of steroid hormones in human urine with HPLC-Q-ToF detection

Dmitrieva, Ekaterina; Темердашев, А. З.; Zorina, Maria; Feng, Yun; Nesterenko, Pavel N.

doi:10.1016/j.jpba.2022.114736

Cited by 12 publications

(4 citation statements)

References 31 publications

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“…In the case of cyanoacetohydrazide, a comparison with hydroxylamine appears most appropriate ( Table 5 ). An optimized condition of derivatization with hydroxylamine was previously reported in [ 22 ]. A lower limit of quantification for oximes and CAH derivatives corresponds to the lowest point of the linear range and presented at Table 5 .…”

Section: Discussionmentioning

confidence: 99%

“…Regardless of the form of steroids determined during the analysis, the quantification of steroid hormones at trace levels necessitates preliminary sample concentration. The most commonly employed techniques for this purpose include liquid-liquid extraction [ 19 , 20 , 21 ], solid-phase extraction [ 22 , 23 , 24 ], and dispersive liquid-liquid microextraction [ 25 , 26 , 27 ]. In addition, it is imperative to consider that performing non-targeted steroid screening, encompassing estrogens, androgens, progestins, and corticosteroids simultaneously, poses significant challenges due to the switching the polarity required during analysis.…”

Section: Introductionmentioning

confidence: 99%

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Cyanoacetohydrazide as a Novel Derivatization Agent for the Determination of UHPLC-HRMS Steroids in Urine

Temerdashev,

Zorina,

Feng

et al. 2024

Molecules

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The possibility of cyanoacetohydrazide usage as a novel derivatizing agent is demonstrated in the presented article, and a comparison with hydroxylamine as the most commonly used reagent is provided. Optimal conditions for steroid derivatization with cyanoacetohydrazide are provided. According to the collected data, the maximum yield of derivatives was observed at pH 2.8 within 70 min at 40 °C with 5 ng/mL limit of detection for all investigated analytes. It was shown that cyanoacetohydrazide derivatives produces both syn- and anti-forms as well as hydroxylamine, and their ratios were evaluated and shown in presented work. An efficiency enchantment from two to up to five times was achieved with a novel derivatization reagent. Its applicability for qualitative analysis of steroids in urine was presented at real samples. Additionally, the reproducible fragmentation of the derivatizing agent in collision-induced dissociation offers opportunities for simplified non-targeted steroidomic screening. Furthermore, cyanoacetohydrazide increases ionization efficiency in positive mode, which can eliminate the need for redundant high-resolution instrument runs required for both positive and negative mode analyses.

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Section: Discussionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Cyanoacetohydrazide as a Novel Derivatization Agent for the Determination of UHPLC-HRMS Steroids in Urine

Temerdashev,

Zorina,

Feng

et al. 2024

Molecules

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“…The analyses of the proposed method used small volumes of sample (1.5 mL), considering that it was not necessary to perform urine dilution, thus reducing possible errors associated with this step. A total preparation time of ≈2 min was needed per sample when the sampling well plate system was operated at maximum capacity, which favors the highthroughput of this method, because multiple samples can be analyzed simultaneously, while the other methods required much longer times, up to 1 h [23,[33][34][35][36][37][38][39][40].…”

Section: Analytical Parameters Of Meritmentioning

confidence: 99%

Polyaniline‐silica doped with oxalic acid as a novel extractor phase in thin film solid‐phase microextraction for determination of hormones in urine

Turazzi

Morés

Carasek

et al. 2023

J of Separation Science

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In this study, different polyanilines were synthesized and evaluated for the determination of three hormones, including 17-β-estradiol, 17-α-ethinylestradiol, and estrone, in urine using a novel methodology based on thin film solidphase microextraction technique, employing the sampling well plate system.The extractor phases, designated as polyaniline doped with hydrochloric acid, polyaniline doped with oxalic acid, polyaniline-silica doped with hydrochloric acid, and polyaniline-silica doped with oxalic acid, were characterized by electrical conductivity measurements, scanning electron microscopy, and Fourier transform infrared spectroscopy. The optimized extraction conditions were composed of 1.5 mL of urine and pH adjusted to 10, with no need to dilute sample and the desorption step, 300 μL of acetonitrile was used. The calibration curves were performed in the sample matrix, with detection and quantification limits ranged from 0.30 to 3.03 μg L −1 and from 1.0 to 10.0 μg L −1 , respectively, with r ≥ 0.9969. The relative recoveries ranged from 71% to 115%, and intraday precision showed values ≤12% and interday ≤20%. The applicability of the method was successfully evaluated, and six urine samples from female volunteers were analyzed. The analytes were not detected or were below the limits of quantification in these samples.

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“…This reagent allows the silylation of even enol groups thus resulting in an increase in the intensity of a molecular ion and consequently in higher sensitivity of analysis. In the case of HPLC determination of steroids, the use of derivatization reagents is less common; however, when their application is required, hydroxylamine can be used [33] as a simple and efficient reagent compatible with aqueous media.…”

Section: Introductionmentioning

confidence: 99%

GC-MS/MS Determination of Steroid Hormones in Urine Using Solid-Phase Derivatization as an Alternative to Conventional Methods

et al. 2022

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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.

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Solid-phase analytical derivatization as a tool for the quantification of steroid hormones in human urine with HPLC-Q-ToF detection

Cited by 12 publications

References 31 publications

Cyanoacetohydrazide as a Novel Derivatization Agent for the Determination of UHPLC-HRMS Steroids in Urine

Cyanoacetohydrazide as a Novel Derivatization Agent for the Determination of UHPLC-HRMS Steroids in Urine

Polyaniline‐silica doped with oxalic acid as a novel extractor phase in thin film solid‐phase microextraction for determination of hormones in urine

GC-MS/MS Determination of Steroid Hormones in Urine Using Solid-Phase Derivatization as an Alternative to Conventional Methods

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