Simultaneous determination of androstenediol 3-sulfate and dehydroepiandrosterone sulfate in human serum using isotope diluted liquid chromatography–electrospray ionization-mass spectrometry

Mitamura, Kuniko; Nagaoka, Yoko; Shimada, Kazutake; Honma, Sato; Namiki, Mikio; Koh, Eitetsu; Mizokami, Atsushi

doi:10.1016/j.jchromb.2003.08.011

Cited by 24 publications

(24 citation statements)

References 25 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…Quality control samples (QCs) containing different concentrations of each analyte were prepared and analyzed. The selected values for each sulfated steroid were in accordance with the expected concentrations reported in the bibliography ( 11,13,14 ) and with the preliminary results found in real samples prior to method evaluation . QCs were always prepared in stripped human serum, because a real serum sample lacking all the sulfated steroids to analyze could not be obtained.…”

Section: Mssupporting

confidence: 84%

“…Additionally, there are two LC-MS assays focused on the analysis of CS in serum ( 11,12 ). Other LC-MSbased methods performed the analysis of androgen sulfates ( 13,14,17 ). Our method is the fi rst to quantify CS in combination with androgen sulfates, PregS, and 17OHPregS in a single run.…”

Section: Msmentioning

confidence: 99%

“…Recent examples can be found in ( 9,10 ). Other methods were developed to analyze only one compound ( 11,12 ) or a limited number of sulfated steroids ( 13,14 ). In 2003, Liu, Griffi ths, and Sjövall ( 15 ) provided a method to obtain a more detailed profi ling of sulfated steroids in human plasma.…”

mentioning

confidence: 99%

See 2 more Smart Citations

Simultaneous quantification of cholesterol sulfate, androgen sulfates, and progestagen sulfates in human serum by LC-MS/MS

Sánchez‐Guijo

Oji

Hartmann

et al. 2015

Journal of Lipid Research

View full text Add to dashboard Cite

Human adrenal glands, and those of some primates, secrete high concentrations of conjugated steroids, particularly 5-androsten-3 ␤ -ol-17-one-3-sulfate [dehydroepiandrosterone sulfate (DHEAS)], which reaches different peripheral tissues through blood ( 1 ). Sulfonation increases the solubility of steroids in water-based biological fl uids such as blood or urine. Sulfated steroids, also known in the literature as steroid sulfates or steroid sulfonates, represent the most abundant fraction of steroids in human blood. Because the physiological activity has been traditionally assigned to the unconjugated steroids, the classical dogma assumes that sulfated steroids are inactive forms of steroids which require sulfate cleavage to be active . In this context, human steroid sulfatase (STS) is the enzyme that desulfates the sulfated steroids to obtain free forms. The complementary reaction, sulfonation, is provided by sulfotransferase enzymes ( Fig. 1 ). This cycle allows for the regulation and excretion of steroids.The concept of steroid sulfates as inactive compounds is under revision. A specifi c transporter for sulfated steroids in the human testis was recently described ( 2 ). Moreover, Abstract Steroids are primarily present in human fl uids in their sulfated forms. Profi ling of these compounds is important from both diagnostic and physiological points of view . Here, we present a novel method for the quantifi cation of 11 intact steroid sulfates in human serum by LC-MS/MS. The compounds analyzed in our method, some of which are quantifi ed for the fi rst time in blood, include cholesterol sulfate, pregnenolone sulfate, 17-hydroxy-pregnenolone sulfate, 16-␣ -hydroxy-dehydroepiandrosterone sulfate, dehydroepiandrosterone sulfate, androstenediol sulfate, androsterone sulfate, epiandrosterone sulfate, testosterone sulfate, epitestosterone sulfate, and dihydrotestosterone sulfate. The assay was conceived to quantify sulfated steroids in a broad range of concentrations, requiring only 300 l of serum. The method has been validated and its performance was studied at three quality controls, selected for each compound according to its physiological concentration. The assay showed good linearity (R 2 > 0.99) and recovery for all the compounds, with limits of quantifi cation ranging between 1 and 80 ng/ml. Averaged intra-day and between-day precisions (coeffi cient of variation) and accuracies (relative errors) were below 10%. The method has been successfully applied to study the sulfated steroidome in diseases such as steroid sulfatase deficiency, proving its diagnostic value. This is, to our best knowledge, the most comprehensive method available for the quantifi cation of sulfated steroids in human blood. -S á nchez-Guijo, A., V. Oji, M.

show abstract

Section: Mssupporting

confidence: 84%

Section: Msmentioning

confidence: 99%

See 1 more Smart Citation

Simultaneous quantification of cholesterol sulfate, androgen sulfates, and progestagen sulfates in human serum by LC-MS/MS

Sánchez‐Guijo

Oji

Hartmann

et al. 2015

Journal of Lipid Research

View full text Add to dashboard Cite

show abstract

“…Incidentally, the charcoal-treated specimens have often been used in endogenous steroid assays as blank matrices (Mitamura et al, 2003;Cawood et al, 2005). The regression lines obtained from the combination of five calibration curves are summarized in slopes were below 1.7%.…”

Section: Calibration Curves Loq and Lodmentioning

confidence: 99%

Studies on neurosteroids XXII. Liquid chromatography–tandem mass spectrometric method for profiling rat brain 3‐oxo‐4‐ene‐neuroactive steroids

Higashi

Nagahama

Mukai

et al. 2007

Biomedical Chromatography

Self Cite

View full text Add to dashboard Cite

A sensitive liquid chromatography-electrospray ionization-tandem mass spectrometric (LC-ESI-MS/MS) method for the simultaneous determination of five 3-oxo-4-ene-neuroactive steroids, i.e. androstenedione, testosterone (T), progesterone (PROG), 20alpha-dihydroprogesterone and 20beta-dihydroprogesterone, in rat brain has been developed and validated. The brain steroids were extracted with methanol-acetic acid, purified using solid-phase extraction cartridges and subjected to LC-ESI-MS/MS. The method does not require derivatization. Deuterium-labeled T and PROG were used as the internal standards, and quantification was based on the selected reaction monitoring mode. This method allowed the reproducible and accurate quantification of the brain neuroactive steroids using 100 mg of tissue; the intra- and inter-assay relative standard deviations were below 4.7 and 4.3%, respectively, and the accuracy values were 97.6-103.2% for all the steroids. The limits of quantitation were 0.1 ng/g tissue for all the steroids. The application of this developed method for the analysis of changes in the brain neuroactive steroid levels by immobilization stress is also presented.

show abstract

“…Slightly lower DHEAS values were observed in BPH (2.6 µM) and PC subjects (1.9 µM) compared to control subjects (4.3 µM) in one study, but sample size was limited (Mitamura et al 2003). Additionally, lower DHEAS levels were associated with an increased risk for aggressive PC (Severi et al 2006).…”

Section: Dheasmentioning

confidence: 91%

Circulating steroid hormone variations throughout different stages of prostate cancer

Snaterse¹,

Visser²,

Arlt³

et al. 2017

Endocrine-Related Cancer

View full text Add to dashboard Cite

Steroid hormones play a central role in the maintenance and progression of prostate cancer. The androgen receptor is the primary driver of tumor cell proliferation and is activated by the androgens testosterone and 5α-dihydrotestosterone. Inhibition of this pathway through medical or surgical castration improves survival in the majority of advanced prostate cancer patients. However, conversion of adrenal androgen precursors and alternative steroidogenic pathways have been found to contribute to tumor progression and resistance to treatment. The emergence of highly accurate detection methods allows us to study steroidogenic mechanisms in more detail, even after treatment with potent steroidogenic inhibitors such as the CYP17A1 inhibitor abiraterone. A clear overview of steroid hormone levels in patients throughout the local, metastatic and castration-resistant stages of prostate cancer and treatment modalities is key toward a better understanding of their role in tumor progression and treatment resistance. In this review,

show abstract

Simultaneous determination of androstenediol 3-sulfate and dehydroepiandrosterone sulfate in human serum using isotope diluted liquid chromatography–electrospray ionization-mass spectrometry

Cited by 24 publications

References 25 publications

Simultaneous quantification of cholesterol sulfate, androgen sulfates, and progestagen sulfates in human serum by LC-MS/MS

Simultaneous quantification of cholesterol sulfate, androgen sulfates, and progestagen sulfates in human serum by LC-MS/MS

Studies on neurosteroids XXII. Liquid chromatography–tandem mass spectrometric method for profiling rat brain 3‐oxo‐4‐ene‐neuroactive steroids

Circulating steroid hormone variations throughout different stages of prostate cancer

Contact Info

Product

Resources

About