Standardized LC–MS/MS based steroid hormone profile-analysis

17β-estradiol (E2) and 17α-ethinyl estradiol (EE2), which are environmental estrogens have been determined with LC-MS in freshwater. Their sensitive analysis needs derivatisation and therefore is very hard to achieve in multiresidue screening. We analysed samples from all the large and some small rivers (River Danube, Drava, Mur, Sava, Tisza and Zala) of the Carpathian Basin and from Lake Balaton. Freshwater was extracted on solid phase and derivatised using dansyl-chloride. Separation was performed on a Kinetex XB-C18 column. Detection was achieved with a benchtop orbitrap mass spectrometer using targeted MS analysis for quantification. Limits of quantification were 0.05 ng/L (MS1) and 0.1 ng/L (MS/MS) for E2, and 0.001 ng/L (MS1) and 0.2 ng/L (MS/MS) for EE2. River samples contained n.d.-5.2 ng/L E2 and n.d.-0.68 ng/L EE2. Average levels of E2 and EE2 were 0.61 and 0.084 ng/L respectively in rivers, water courses and Lake Balaton together, but not counting city canal water. EE2 was less abundant, but it was still present in almost all of the samples. In beach water samples from Lake Balaton we measured 0.076-0.233 E2 and n.d.-0.133 EE2. A relative high amount of EE2 was found in river Zala (0.68 ng/L) and in Hévíz-Páhoki canal (0.52 ng/L), which are both in the catchment area of Lake Balaton (Hungary). HighlightsMethod is proposed for simultaneous determination of 17β-estradiol and 17α-ethinyl estradiol. Derivatization is necessary to reach low LOQ. Low ng/L presence of estrogens in selected European Rivers has been detected.

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“…tSIM scan ranges were 506.0-506. (Koal et al 2012) was found 7.5 µg/L. LOQ for EE2 detected as m/z 295.16 (MS1) was 20 ng/L.…”

Section: Hplc-ms Analysis Hplc-ms Was Carried Out On a Q-exactive Orbmentioning

confidence: 92%

β-Estradiol and ethinyl-estradiol contamination in the rivers of the Carpathian Basin

Avar

Zrínyi²,

Maász

et al. 2016

Environ Sci Pollut Res

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“…Samples were analyzed using Absolute IDQ Stero17 Kit produced by Biocrates Life Sciences AG (Innsbruck, Austria) according to the validated protocol supplied by the manufacturer. Steroids were analyzed in positive ionization (for DHEA-S both positive and negative) in multiple reaction monitoring mode [10]. The intra-and interassay variability did not exceed 11.5%.…”

Section: Biochemical Measurementsmentioning

confidence: 99%

Total testosterone to dihydrotestosterone ratio assessed by LC-MS/MS predicts a worse metabolic profile not only in PCOS patients

et al. 2017

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Objectives: Total testosterone/dihydrotestosterone ratio (TT/DHT) was found to determine metabolic risk in polycystic ovary syndrome (PCOS). The aim of this study was to analyze whether (TT/DHT) may be helpful in predicting metabolic risk not only in PCOS patients but also in healthy women. Material and methods:Total testosterone (TT), dihydrotestosterone (DHT), androstendione and dehydroepiandrosterone sulphate (DHEA-S) were measured by LC-MS/MS in 36 women with PCOS and in 29 age-matched controls without clinical hyperandrogenism. In all participants, anthropometric data, lipids, adipose tissue percent (%fat), HOMA-IR were also assessed. Results:The studied groups were not different in terms of age, BMI, waist circumference, %fat and HOMA-IR. In the patients group, mean TT and androstendione levels were significantly higher as compared to controls (1.4 nmol/L vs. 1.0 nmol/L, P < 0.001) and (6.6 nmol/L vs. 4.9 nmol/L, P < 0.01), respectively. In the patients group, mean TT/DHT ratio was significantly higher compared to controls (3.6 vs. 2.7, P < 0.01) and correlated with BMI (r = 0.37, P < 0.05), waist circumference (r = 0.44, P < 0.01), %fat (r = 0.30, P < 0.05), as well as with insulin levels (r = 0.38, P < 0.05) and HOMA-IR (r = 0.44, P < 0.05). The association between TT/DHT ratio and unfavorable metabolic parameters was also seen in controls. Conclusion:Total testosterone/dihydrotestosterone ratio assessed by LC-MS/MS correlates with a worse metabolic profile not only in PCOS patients, but also in healthy women.

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“…Furthermore, the analytical portfolio is quickly extended by clinically relevant compounds like steroid hormones (Koal et al, 2012;Ackermans & Endert, 2014), bile acids (Griffiths & Sjövall, 2010), catecholamines (Bicker et al, 2013), and others.…”

Section: A C C E P T E D Accepted Manuscriptmentioning

confidence: 99%