Quantification of steroid hormones in human urine by DLLME and UHPLC-HRMS detection

Dmitrieva, Ekaterina; Темердашев, А. З.; Azaryan, A. A.; Gashimova, Elina

doi:10.1016/j.jchromb.2020.122390

Cited by 15 publications

(12 citation statements)

References 32 publications

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“…The presented study was compared with two articles which used DLLME method for the determination of steroid hormones [27,28]. In published article [27] the following results were obtained: 1 -steroid hormones in this article are cortisone, cortisol, prednisolone, corticosterone, testosterone, 17a-methyltestosterone, epitestosterone and progesterone.…”

Section: Comparison Presented Study With Other Reported Methodsmentioning

confidence: 83%

Dispersive liquid-liquid microextraction followed by high-performance liquid chromatography as an efficient and sensitive technique for determination of nandrolone and testosterone in human urine

Rezaee

2023

AChrom

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Dispersive liquid-liquid microextraction (DLLME) and high performance liquid chromatography – UV detection was presented for extraction and determination of nandrolone and testosterone in human urines. Chloroform at microliter volume level and acetonitrile were used as extraction and dispersive solvents, respectively. The main advantages of method are high speed, high enrichment factor, high recovery, good repeatability and extraction solvent volume at µL level. The influence of several variables (e.g. type and volume of disperser and extraction solvents, ionic strength, etc.) on the performance of the sample preparation step was carefully evaluated. Under the optimum conditions, the calibration graphs were linear in the range of 5–500 μg L−1 with detection limit of 2.5 μg L−1 for both of them. The relative standard deviation (R.S.D.s) for five replicate measurements of nandrolone and testosterone were 9.4% and 8.8%, respectively. The relative recoveries of nandrolone and testosterone in urine sample at spiking level of 25.0 μg L−1 are ranged between 86.4% and 98%. DLLME combined with HPLC-UV is a fast, simple and efficient method for the determination of nandrolone and testosterone in human urines.

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Section: Comparison Presented Study With Other Reported Methodsmentioning

confidence: 83%

Dispersive liquid-liquid microextraction followed by high-performance liquid chromatography as an efficient and sensitive technique for determination of nandrolone and testosterone in human urine

Rezaee

2023

AChrom

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“…Thus, a sensitive, simple, and reproducible method was developed for the determination of ketosteroids. Derivatization with hydroxylamine made it possible to significantly increase the sensitivity of the method for most compounds in comparison with our previous work [8], especially for estrone. An analysis of real samples showed a possibility of using the proposed method for the determination of ketosteroids.…”

Section: Discussionmentioning

confidence: 90%

“…It should be noted that, in the analysis of real samples before the microextraction procedure, glucuronides were deconjugated under the conditions optimized by us earlier [8]: 30 min at 50°C in the presence of a phosphate buffer solution (pH 6.5) and enzyme β-glucuronidase from E. coli.…”

Section: Articlesmentioning

confidence: 99%

“…The results of the real-time determination of steroids can fluctuate because of the episodic hormone secretion [5,6] and also circadian rhythms [7], while the composition of urine is not subjected to such fluctuations. Other advantages of urine as a test sample are the non-invasiveness of the procedure and the ease of obtaining large sample volumes [8].…”

mentioning

confidence: 99%

“…Various methods of the preparation of urine samples for analysis are used: liquid-liquid extraction [11][12][13], stir bar sorptive extraction [14], on-line intube solid-phase microextraction [15], automated solid-phase extraction [16], dispersive liquid-liquid microextraction (DLLME) [8], and others [17]. Among the listed methods, the most promising is DLLME because of its simplicity, high concentration factors, and compliance with the criteria of "green chemistry" [18].…”

mentioning

confidence: 99%

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Determination of Ketosteroids in Human Urine Using Dispersive Liquid-Liquid Microextraction and Ultra High-Performance Liquid Chromatography-High Resolution Mass Spectrometry

2021

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A method is proposed for the determination of some ketosteroids in human urine, including enzymatic hydrolysis using β-glucuronidase from E. coli followed by dispersive liquid-liquid microextraction, derivatization of analytes with hydroxylamine, and detection by reversed-phase ultra-HPLC–quadrupole time-of-flight mass spectrometry. Optimization of extraction and derivatization conditions of the studied compounds made it possible to find that the highest recoveries were achieved using an acetone–chloroform mixture as a dispersant and an extractant, and the completeness of the derivatization reaction was achieved by thermostating the sample at 70°C for 90 min. The proposed method has high sensitivity (limits of detection in the range of 0.1–0.25 ng/mL) and a wide linearity range.

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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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Quantification of steroid hormones in human urine by DLLME and UHPLC-HRMS detection

Cited by 15 publications

References 32 publications

Dispersive liquid-liquid microextraction followed by high-performance liquid chromatography as an efficient and sensitive technique for determination of nandrolone and testosterone in human urine

Dispersive liquid-liquid microextraction followed by high-performance liquid chromatography as an efficient and sensitive technique for determination of nandrolone and testosterone in human urine

Determination of Ketosteroids in Human Urine Using Dispersive Liquid-Liquid Microextraction and Ultra High-Performance Liquid Chromatography-High Resolution Mass Spectrometry

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

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