Analysis by LC–MS/MS of endogenous steroids from human serum, plasma, endometrium and endometriotic tissue

Häkkinen, Merja R.; Heinosalo, Taija; Saarinen, Niina M.; Linnanen, Tero; Voutilainen, Raimo; Lakka, Timo A.; Jääskeläinen, Jarmo; Poutanen, Matti; Auriola, Seppo

doi:10.1016/j.jpba.2018.01.034

Cited by 60 publications

(64 citation statements)

References 16 publications

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“…Such deficient traceability inevitably will reduce the recognition of the results from these methods. Another problem is that these methods for steroid metabolome analysis cannot detect important estrogens such as estradiol and estriol in a single analysis (14,16) because the estrogens are often detected under negative mode, which is incompatible with the other steroids (1). In addition, these methods require a large sample volume (10,14,17), which reduces the applicability of the method.…”

Section: Lc/ms/ms Methods For Analyzing Steroid Metabolome 581mentioning

confidence: 99%

An LC/MS/MS method for analyzing the steroid metabolome with high accuracy and from small serum samples

Yuan

Wang³

et al. 2020

Journal of Lipid Research

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Analyzing global steroid metabolism in humans can shed light on the etiologies of steroid-related diseases. However, existing methods require large amounts of serum and lack the evaluation of accuracy. Here, we developed an LC/MS/MS method for the simultaneous quantification of 12 steroid hormones: testosterone, pregnenolone, progesterone, androstenedione, corticosterone, 11-deoxycortisol, cortisol, 17-hydroxypregnenolone, 17-hydroxyprogesterone, dehydroepiandrosterone, estriol, and estradiol. Steroids and spiked internal standards in 100 μl serum were extracted by protein precipitation and liquid-liquid extraction. The organic phase was dried by evaporation, and isonicotinoyl chloride was added for steroid derivatization, followed by evaporation under nitrogen and redissolution in 50% methanol. Chromatographic separation was performed on a reverse-phase PFP column, and analytes were detected on a triple quadrupole mass spectrometer with ESI. The lower limits of quantification ranged from 0.005 ng/ml for estradiol to 1 ng/ml for cortisol. Apparent recoveries of steroids at high, medium, and low concentrations in quality control samples were between 86.4% and 115.0%. There were limited biases (−10.7% to 10.5%) between the measured values and the authentic values, indicating that the method has excellent reliability. An analysis of the steroid metabolome in pregnant women highlighted the applicability of the method in clinical serum samples. We conclude that the LC/MS/MS method reported here enables steroid metabolome analysis with high accuracy and reduced serum consumption, indicating that it may be a useful tool in both clinical and scientific laboratory research.

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Section: Lc/ms/ms Methods For Analyzing Steroid Metabolome 581mentioning

confidence: 99%

An LC/MS/MS method for analyzing the steroid metabolome with high accuracy and from small serum samples

Yuan

Wang³

et al. 2020

Journal of Lipid Research

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“…In the initial reports, some analytical methods based on chromatography have been proposed to measure estrogens in urine samples and other biological samples [192][193][194][195][196][197]. However, due to the trace levels of estrogens in real samples, and the massive complexity of these matrixes [198], which can block compatibility with the analysis instrument, an excellent sample preparation material is useful before HPLC analysis of estrogens.…”

Section: Hormonesmentioning

confidence: 99%

Recent Progress on Luminescent Metal-Organic Framework-Involved Hybrid Materials for Rapid Determination of Contaminants in Environment and Food

et al. 2020

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The high speed of contaminants growth needs the burgeoning of new analytical techniques to keep up with the continuous demand for monitoring and legislation on food safety and environmental pollution control. Metal-organic frameworks (MOFs) are a kind of advanced crystal porous materials with controllable apertures, which are self-assembled by organic ligands and inorganic metal nodes. They have the merits of large specific surface areas, high porosity and the diversity of structures and functions. Latterly, the utilization of metal-organic frameworks has attracted much attention in environmental protection and the food industry. MOFs have exhibited great value as sensing materials for many targets. Among many sensing methods, fluorometric sensing is one of the widely studied methods in the detection of harmful substances in food and environmental samples. Fluorometric detection based on MOFs and its functional materials is currently one of the most key research subjects in the food and environmental fields. It has gradually become a hot research direction to construct the highly sensitive rapid sensors to detect harmful substances in the food matrix based on metal-organic frameworks. In this paper, we introduced the synthesis and detection application characteristics (absorption, fluorescence, etc.) of metal-organic frameworks. We summarized their applications in the MOFs-based fluorometric detection of harmful substances in food and water over the past few years. The harmful substances mainly include heavy metals, organic pollutants and other small molecules, etc. On this basis, the future development and possible application of the MOFs have prospected in this review paper.

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“…Indeed, the value of MS assays in obtaining novel data in both clinical specimens and preclinical models is well demonstrated (e.g. Vandenput et al 2007, Harwood & Handelsman 2009, Arlt et al 2011, Keski-Rahkonen et al 2011, Keski-Rahkonen et al 2013, Tamae et al 2013, Ke et al 2015, Nilsson et al 2015, Boggs et al 2016, Snaterse et al 2016, Zang et al 2017, Häkkinen et al 2018. The discussion and debate for the benefits and drawbacks of steroid hormone analysis using either MS or immunoassay methodology has been active, and well-summarized in recent reviews (Taylor et al 2015, Cross & Hornshaw 2016, Handelsman 2017, Wudy et al 2018.…”

Section: Development Of Highly Sensitive Mass Spectrometric Assays Fomentioning

confidence: 99%

“…Poor ionization properties of certain steroids have been one of the challenges in some MS methods, leading to low sensitivity of these assays. Thus, derivatization of the steroids has often been a prerequisite procedure for improving the sensitivity (Keski-Rahkonen et al 2011, Häkkinen et al 2018, but it also increases the complexity, reproducibility and the workload of the method. Nevertheless, the current LC-MS/MS-based assays without derivatization provide very high sensitivity with reference level specificity, also with multianalyte methods; however, neither with MS methodology is it simple to guarantee the right or accurate result of certain steroid.…”

Section: Development Of Highly Sensitive Mass Spectrometric Assays Fomentioning

confidence: 99%

“…Especially, the deconjugation of steroid conjugates via solvolysis or hydrolysis during the process and the conversion of steroids to their metabolites must be carefully tested for proper quantitation of steroids using MS assays. Taking the issues above into a count, with the state-of-the-art GCand LC-MS/MS techniques, we can now measure several androgens with methods being sensitive enough to most applications both in human and preclinical studies (see, for example Harwood & Handelsman 2009, Nilsson et al 2015, Häkkinen et al 2018. However, different assay conditions are often needed for the maximal sensitivity for different steroids, and the techniques used need to be selected based on the preferred sensitivity for the steroids of highest interest (Table 1, for examples).…”

Section: Development Of Highly Sensitive Mass Spectrometric Assays Fomentioning

confidence: 99%

See 1 more Smart Citation

Applying mass spectrometric methods to study androgen biosynthesis and metabolism in prostate cancer

Knuuttila

Hämäläinen

Poutanen

2019

Journal of Molecular Endocrinology

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Recent development of gas chromatography and liquid chromatography-tandem mass spectrometry (GC-MS/MS, LC-MS/MS) has provided novel tools to define sex steroid concentrations. These new methods overcome several of the problems associated with immunoassays for sex steroids. With the novel MS-based applications we are now able to measure small concentrations of the steroid hormones reliably and with high accuracy in both body fluids and tissue homogenates. The sensitivity of the tandem mass spectrometry assays allows us also for the first time to reliably measure picomolar or even femtomolar concentrations of estrogens and androgens. Furthermore, due to a high sensitivity and specificity of MS technology, we are also able to measure low concentrations of steroid hormones of interest in the presence of pharmacological concentration of other steroids and structurally closely related compounds. Both of these features are essential for multiple preclinical models for prostate cancer. The MS assays are also valuable for the simultaneous measurement of multiple steroids and their metabolites in small sample volumes in serum and tissue biopsies of prostate cancer patients before and after drug interventions. As a result, novel information about steroid hormone synthesis and metabolic pathways in prostate cancer has been obtained. In our recent studies, we have extensively applied a GC-MS/MS method to study androgen biosynthesis and metabolism in VCaP prostate cancer xenografts in mice. In the present review, we shortly summarize some of the benefits of the GC-MS/MS and novel LC-MS/ MS assays, and provide examples of their use in defining novel mechanisms of androgen action in prostate cancer. Journal of Molecular Endocrinology(2019) 62, R255-R267

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Analysis by LC–MS/MS of endogenous steroids from human serum, plasma, endometrium and endometriotic tissue

Cited by 60 publications

References 16 publications

An LC/MS/MS method for analyzing the steroid metabolome with high accuracy and from small serum samples

An LC/MS/MS method for analyzing the steroid metabolome with high accuracy and from small serum samples

Recent Progress on Luminescent Metal-Organic Framework-Involved Hybrid Materials for Rapid Determination of Contaminants in Environment and Food

Applying mass spectrometric methods to study androgen biosynthesis and metabolism in prostate cancer

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