Simultaneous determination of thirteen different steroid hormones using micro UHPLC-MS/MS with on-line SPE system

Márta, Zoltán; Bobály, Balázs; Fekete, Jenő; Magda, Balázs; Imre, Tı́mea; Mészáros, Katalin; Bálint, Mária; Szabó, Pál

doi:10.1016/j.jpba.2017.12.014

Cited by 38 publications

(24 citation statements)

References 36 publications

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“…For this purpose there are several extraction techniques such as liquid‐liquid extraction (LLE), solid phase extraction (SPE), pressurized fluid extraction (PFE) and supercritical fluid extraction (SFE) , among which SPE has received special attention because this technique can be coupled online with HPLC‐MS/MS systems . The on‐line SPE is an efficient fully automatic sample preparation that has several advantages such as: reduced errors and analysis time; smaller amount of samples and organic solvents is necessary; reduced the contact to hazardous reagents and infectious materials; lower detection limits; improve method sensitivity and robustness when compared to off‐line SPE sample preparation .…”

Section: Introductionmentioning

confidence: 99%

Online fully automated SPE‐HPLC‐MS/MS determination of ceftiofur in bovine milk samples employing a silica‐anchored ionic liquid as sorbent

et al. 2018

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Solid-phase extraction coupled online with high performance liquid chromatography and tandem mass spectrometry was successfully applied to determine low concentrations of ceftiofur antibiotic in bovine milk samples. A silica-anchored ionic liquid was applied as sorbent material to be used as extraction phase in the proposed online system. The material was characterized by Fourier transform infrared spectroscopy and scanning electron microscopy. In order to improve the system reproducibility, the following experimental parameters were optimized: organic solvent percentage, time and sample loading flow rate. Subsequently, the method was validated presenting satisfactory results as adequate selectivity, good linearity and correlation coefficient higher than 0.98. The limit of detection and quantification were 0.1 and 0.7 μg/L, respectively. The precision of the methodology was evaluated as repeatability and intermediate precision, with relative standard deviation values lower than 15%. The accuracy of the method ranged from 72.8 to 137% and the minimum and maximum recovery values were 73.4 and 111.3%, respectively. After the validation, seven milk samples were analyzed and although ceftiofur was not detected in any of them the method was demonstrated to be efficient when applied to the analysis of milk samples fortified with the pollutant of interest.

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Section: Introductionmentioning

confidence: 99%

Online fully automated SPE‐HPLC‐MS/MS determination of ceftiofur in bovine milk samples employing a silica‐anchored ionic liquid as sorbent

et al. 2018

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“…Naldi and co-workers (2016) designed and validated a fully automated method combining an online SPE with LC-MS/MS for simultaneous analysis of the free and conjugated forms of selected steroids in urine and various types of water (sewage water, river water, etc.). A similar arrangement may be seen in works concerned with the analysis of other matrices; for example, human saliva or plasma [53,108]. Online SPE has several advantages compared to the offline approach [29,53].…”

Section: Sample Preparation For Lc-msmentioning

confidence: 89%

Analytical Methods for the Determination of Neuroactive Steroids

et al. 2021

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Neuroactive steroids are a family of all steroid-based compounds, of both natural and synthetic origin, which can affect the nervous system functions. Their biosynthesis occurs directly in the nervous system (so-called neurosteroids) or in peripheral endocrine tissues (hormonal steroids). Steroid hormone levels may fluctuate due to physiological changes during life and various pathological conditions affecting individuals. A deeper understanding of neuroactive steroids’ production, in addition to reliable monitoring of their levels in various biological matrices, may be useful in the prevention, diagnosis, monitoring, and treatment of some neurodegenerative and psychiatric diseases. The aim of this review is to highlight the most relevant methods currently available for analysis of neuroactive steroids, with an emphasis on immunoanalytical methods and gas, or liquid chromatography combined with mass spectrometry.

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“…For obtaining MIPs based on silica gel, the modified method described in the literature was used . In the first step, silica gel (5 g) was dried in a vacuum reactor at 140°C for 24 h. After the physically absorbed water was removed from the silica gel, without contact with the environment, 40 mL of anhydrous toluene, 4 mL of γ‐MAPS, and 0.8 mL of triethylamine were introduced.…”

Section: Methodsmentioning

confidence: 99%

“…Therefore, it is necessary to concentrate and purify the analytes present in water samples. Many methods have been proposed for extraction of hormones from an aqueous matrix, such as SPE , ultrasonic liquid extraction , dispersive‐SPE sorbent , micro‐SPE , molecularly imprinted solid‐phase extraction (MISPE) , magnetic‐SPE , stir bar sorptive extraction , SPME , stir cake sorptive extraction , fabric phase sorptive extraction and LLE. Due to the low cost of analysis and high sample recovery, the most commonly used technique for concentration and purification of such samples is SPE; however, popular sorbents are characterized by low selectivity that leads to simultaneous extraction of matrix elements .…”

Section: Introductionmentioning

confidence: 99%

Molecularly imprinted polymer film grafted from porous silica for efficient enrichment of steroid hormones in water samples

Szczukocki

Krawczyk

Juszczak

et al. 2019

J of Separation Science

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Steroid hormones as endocrine disrupting compounds can interfere with the functioning of hormonal systems of organisms and thus affect the health and reproduction of humans and wildlife. Unfortunately, these types of harmful endocrine disrupting compounds have been found in a variety of environmental samples at very low concentrations. Therefore, a simple, fast, and efficient method for enrichment of water samples is needed. A molecularly imprinted solid‐phase extraction combined with high performance liquid chromatography coupled with diode array detection was developed for the determination of six steroid hormones, such as estrone, 17‐β‐estradiol, estriol, 17‐α‐ethinylestradiol, progesterone, and testosterone in water samples. The recoveries obtained in the proposed method were in the range of 78.7–101.3%. Matrix effect below 20% suggests that the quantitative and qualitative results of the analysis were not significantly affected by the matrix. The results show that molecularly imprinted polymers based on spherical silica gel had the potential to be a highly innovative and selective sorbent. The proposed method was proved to be applicable for molecularly imprinted solid‐phase extraction in selective and reliable extraction and enrichment of steroid hormones in environmental water samples.

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Simultaneous determination of thirteen different steroid hormones using micro UHPLC-MS/MS with on-line SPE system

Cited by 38 publications

References 36 publications

Online fully automated SPE‐HPLC‐MS/MS determination of ceftiofur in bovine milk samples employing a silica‐anchored ionic liquid as sorbent

Online fully automated SPE‐HPLC‐MS/MS determination of ceftiofur in bovine milk samples employing a silica‐anchored ionic liquid as sorbent

Analytical Methods for the Determination of Neuroactive Steroids

Molecularly imprinted polymer film grafted from porous silica for efficient enrichment of steroid hormones in water samples

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