High performance liquid chromatography/ion-trap mass spectrometry for separation and simultaneous determination of ethynylestradiol, gestodene, levonorgestrel, cyproterone acetate and desogestrel

Matějíček, David; Kubáň, Vlastimil

doi:10.1016/j.aca.2007.02.028

Cited by 57 publications

(22 citation statements)

References 20 publications

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“…These limits are equal or slightly higher than those found by other authors [34][35][36][37] because the demands set by validation criteria defined by accreditation process because EPAL laboratory is accredited. For these reason, all routine procedures must be validated according national and international procedures [28][29][30][31][32][33].…”

Section: Matrix Effect and Methods Detection Limits (Mdl)contrasting

confidence: 45%

Simultaneous Determination of Ten Endocrine Hormone Disrupters in Water Using SPE/LC-(ESI)MS-MS

Henriques¹,

Cardoso²,

Rodrigues³

et al. 2010

JWARP

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The aim of this study was developed and validated an analytical method based on liquid chromatography and tandem mass spectrometry after solid phase extraction to monitorizing ten endocrine hormone disrupters in Lisbon drinking water system. Natural and synthetic hormones (17-β-estradiol, ethinylestradiol, estriol, estrone, progesterone, mestranol and diethylstilbestrol) and some industrial products (4-n-nonylphenol, 4-tert-octylphenol and bisphenol A) were studied. Mass spectrometer detection parameters were optimized, such as the best conditions for the precursor ion formation, namely cone voltage, when applying negative and positive electrospray ionization, and also collision energy for MRM1 and MRM2 transitions. The best conditions of the solid phase extraction (SPE) using Waters Oasis HLB (6 mL, 200 mg) and Isolute C18 (EC) (6 ml, 1000 mg) were also optimized. The method was validated through the application of several statistical tests and the uncertainty estimation of the analytical assay. This method showed a very good linear range for all the studied analytes with determination coefficients (r 2 ) between 0.9962 and 0.9999 and coefficients of variation lower than 4%. There were no significant differences between recoveries obtained with the studied matrices, like groundwater, surface water and water for human consumption. In these matrices, the recovery values varied between 32 and 95%. The limits of method detection were between 0.28 and 22 ng/L. The validated method was applied for the analysis of water samples from the EPAL (Empresa Portuguesa das Águas Livres, S.A.) water supply system including tap water, spring water, groundwater, and river water. Some target compounds (bisphenol A, progesterone, 4-tert-octylphenol, and 4-n-nonylphenol) were found in trace amounts in analysed waters.

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Section: Matrix Effect and Methods Detection Limits (Mdl)contrasting

confidence: 45%

Simultaneous Determination of Ten Endocrine Hormone Disrupters in Water Using SPE/LC-(ESI)MS-MS

Henriques¹,

Cardoso²,

Rodrigues³

et al. 2010

JWARP

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“…Recently, high performance liquid chromatography with mass spectrometric (LC/MS) methods have been favored over GC/MS detection as they do not require a derivatization step prior to analysis. The LODs reported for LC/MS or LC/MS/MS analyses of water-associated hormones range between 0.02 and 1.0 ng/L [19][20][21][22][23]. Accordingly, liquid chromatography with tandem mass spectrometric detection was demonstrated to be superior to immunoassay methods or GC/MS in terms of selectivity, sensitivity, simplicity and analytical throughput.…”

Section: Introductionmentioning

confidence: 99%

“…Liquid-liquid extraction (LLE) and solid-phase extraction (SPE) [19,21,23] are most common extraction methods used for the determination of steroid hormones. However, LLE requires large volumes of organic solvents and additional clean-up steps, and although SPE requires small volumes of organic solvents, the manual version is tedious and time consuming.…”

Section: Introductionmentioning

confidence: 99%

Simultaneous determination of 15 steroidal oral contraceptives in water using solid-phase disk extraction followed by high performance liquid chromatography–tandem mass spectrometry

Sun

Yong

Chu

et al. 2009

Journal of Chromatography A

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a b s t r a c tA rapid, accurate and sensitive method for simultaneous determination of 15 steroidal hormones including four estrogens (estrone, 17␤-estradiol, 17␣-ethynylestradiol, estriol) and eleven progestogens (17␤-estradiol-3-benzoate, 19-norethindrone, gestodene, levonorgestrel, medroxyprogesterone, cyproterone acetate, megestrol-17-acetate, progesterone, norethindrone acetate, chlormadinone-17-acetate, and hydroxy progesterone caproate) in environmental waters was developed by coupling solid-phase disk extraction (SPDE) to ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with electrospray ionization. Among three types of extraction tested (C 8 SPDE, C 18 SPDE and C 18 SPE), the most satisfactory result was achieved using C 18 SPDE for its satisfactory recovery (75.6 to 101.4%) and short extraction time (15 min for 1 L deionised water). The validity of this method was investigated and good analytical performance for all the analytes was obtained, including low limits of method detection (0.5-3.4 ng/L) and excellent linear dynamic range (1.0-50.0 ng/L). The method was applied to determine the steroidal hormones in 10 environmental waters including tap water, river water, lake water and waste water in Beijing. No progestogen was detected in all samples and estrone, estriol, 17␣-ethynylestradiol were found in most samples at levels between 1.8 and 127.9 ng/L.

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“…The LODs reported for LC-ESI-MS and LC-ESI-CID-MS/MS ranged from 0.02 to 1.0 ng/L when analyzing water borne hormones [33][34][35][36][37]. LC-ESI-CID-MS/MS detection was found to be advantageous over immunoassay methods or GC-MS because it is sensitive and compatible for conjugated steroids [38,39].…”

Section: Introductionmentioning

confidence: 89%

Multiplex quantification of lamprey specific bile acid derivatives in environmental water using UHPLC–MS/MS

Wang

Brant

et al. 2011

Journal of Chromatography B

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High performance liquid chromatography/ion-trap mass spectrometry for separation and simultaneous determination of ethynylestradiol, gestodene, levonorgestrel, cyproterone acetate and desogestrel

Cited by 57 publications

References 20 publications

Simultaneous Determination of Ten Endocrine Hormone Disrupters in Water Using SPE/LC-(ESI)MS-MS

Simultaneous Determination of Ten Endocrine Hormone Disrupters in Water Using SPE/LC-(ESI)MS-MS

Simultaneous determination of 15 steroidal oral contraceptives in water using solid-phase disk extraction followed by high performance liquid chromatography–tandem mass spectrometry

Multiplex quantification of lamprey specific bile acid derivatives in environmental water using UHPLC–MS/MS

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