LC–MS/MS coupled with immunoaffinity extraction for determination of estrone, 17β-estradiol and estrone 3-sulfate in human plasma

Hosogi, Jun; Tanaka, Hideyuki; Fujita, Kazuhiro; Kuwabara, Takashi; Ikegawa, Shigeo; Kobayashi, Norihiro; Mano, Nariyasu; Goto, Junichi

doi:10.1016/j.jchromb.2009.08.010

Cited by 38 publications

(14 citation statements)

References 20 publications

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“…In particular analytes that are present at in the picomolar range are attractive candidates for IAC coupled to LC-MS/MS. A recent clinical example is the use of IAC in the determination of low circulating levels of estrone, 17␤-estradiol and estrone-3-sulphate in human plasma [34]. The authors could show similar detection sensitivity for 17␤-estradiol to a reference measurement procedure using SPE followed by derivatization with dansyl chloride prior to LC-MS/MS [35].…”

Section: Sample Preparationmentioning

confidence: 97%

The role of liquid chromatography–tandem mass spectrometry in the clinical laboratory

Ouweland

Kema²

2012

Journal of Chromatography B

127

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Section: Sample Preparationmentioning

confidence: 97%

The role of liquid chromatography–tandem mass spectrometry in the clinical laboratory

Ouweland

Kema²

2012

Journal of Chromatography B

127

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“…LC/MS/MS methodology is not as challenging but endogenous estrogens are not effectively ionized using conventional electrospray ionization (ESI)‐ or atmospheric pressure chemical ionization (APCI)‐based methodology. This has restricted the use of this conventional methodology to samples with higher concentrations of plasma and serum estrogens . In order to use ESI‐ MS or APCI‐MS it has been necessary to enhance the ionization characteristics of estrogens by converting them into suitable derivatives.…”

Section: Discussionmentioning

confidence: 99%

Liquid chromatography/mass spectrometry of pre‐ionized Girard P derivatives for quantifying estrone and its metabolites in serum from postmenopausal women

Rangiah

Shah

Vachani

et al. 2011

Rapid Comm Mass Spectrometry

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An ultrasensitive stable isotope dilution liquid chromatography/selected reaction monitoring/mass spectrometry (LC-SRM/MS) assay has been developed for serum estrone, 16α-hydroxyestrone, 4-methoxyestrone, and 2-methoxyestrone. The enhanced sensitivity was obtained by the use of Girard P (GP) pre-ionized derivatives coupled with microflow LC. The limit of detection for each estrogen using 0.5 mL of serum was 0.156 pg/mL and linear standard curves were obtained up to 20 pg/mL. Serum samples from 20 postmenopausal women (10 lifetime non-smokers and 10 current smokers) were analyzed using this new assay. Mean serum concentrations of estrone and 2-methoxyestrone were 14.06 pg/mL (± 1.56 pg/mL) and 3.30 pg/mL (± 1.00 pg/mL), respectively, for the 20 subjects enrolled in the study. The mean estrone concentration determined by our ultrasensitive and highly specific assay was significantly lower than that reported for the control groups in most previous breast cancer studies of postmenopausal women. In addition (and contrary to many reports) serum 16α-hydroxyestrone was not detected in any of the subjects, and 4-methoxyestrone was detected in only one of the subjects. Furthermore, there were no significant differences in the mean serum concentrations of estrone and 2-methoxyestrone or the ratio of serum 2-methoxyestrone to estrone between the non-smoking and smoking groups. Interestingly, the one subject with measurable serum 4-methoxyestrone (2.3 pg/mL) had the lowest estrone and 2-methoxyestrone concentrations. Using this assay it will now be possible to obtain definitive information on the levels of serum estrone, 4-methoxyestrone, and 2-methoxyestrone in studies of cancer risk using small serum volumes available from previous epidemiology studies.

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“…On the other hand methods based on high‐performance liquid chromatography (HPLC) with electrochemical (Yamada, Yoshizawa, & Hayase, ) and fluorescence (Yilmaz & Kadioglu, ) detection have very low sensitivity (≥2.4 ng/mL) and require very long analysis time (≥15 min). Liquid chromatography–tandem mass spectrometry (LC–MS/MS) has proved to be a better alternative to analyze steroids including E2 in clinical practice (Ferretti et al, ; Fiers et al, ; Gaudl et al, ; Hosogi et al, ; Pauwels et al, ; Wooding et al, ). However, owing to the lack of ionizable groups in estrogens, derivatization is required to improve the sensitivity by introducing charged groups which can promote better ionization efficiency and fragmentation in MS and also for improved retention in chromatography.…”

Section: Introductionmentioning

confidence: 99%

Ultra‐performance liquid chromatography–tandem mass spectrometry assay for determination of plasma nomegestrol acetate and estradiol in healthy postmenopausal women

Nair

Patel

Sanyal

et al. 2017

Biomedical Chromatography

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A highly sensitive and selective ultra-performance liquid chromatography-tandem mass spectrometry method is described for the simultaneous determination of nomegestrol acetate (NOMAC), a highly selective progestogen, and estradiol (E2), a natural estrogen in human plasma. NOMAC was obtained from plasma by solid-phase extraction, while E2 was first separated by liquid-liquid extraction with methyl tert-butyl ether followed by derivatization with dansyl chloride. Deuterated internal standards, NOMAC-d5 and E2-d4 were used for better control of extraction conditions and ionization efficiency. The assay recovery of the analytes was within 90-99%. The analytes were separated on UPLC BEH C (50 × 2.1 mm, 1.7 μm) column using a mobile phase comprising of acetonitrile and 3.0 mm ammonium trifluoroacetate in water (80:20, v/v) with a resolution factor (R ) of 3.21. The calibration curves were linear from 0.01 to 10.0 ng/mL for NOMAC and from 1.00 to 1000 pg/mL for E2, respectively. The intra- and inter-batch precision was ≤5.8% and the accuracy of quality control samples ranged from 96.7 to 103.4% for both analytes. The practical applicability of the method is demonstrated by analyzing samples from 18 healthy postmenopausal women after oral administration of 2.5 mg nomegestrol acetate and 1.5 mg estradiol film-coated tablets under fasting.

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LC–MS/MS coupled with immunoaffinity extraction for determination of estrone, 17β-estradiol and estrone 3-sulfate in human plasma

Cited by 38 publications

References 20 publications

The role of liquid chromatography–tandem mass spectrometry in the clinical laboratory

The role of liquid chromatography–tandem mass spectrometry in the clinical laboratory

Liquid chromatography/mass spectrometry of pre‐ionized Girard P derivatives for quantifying estrone and its metabolites in serum from postmenopausal women

Ultra‐performance liquid chromatography–tandem mass spectrometry assay for determination of plasma nomegestrol acetate and estradiol in healthy postmenopausal women

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