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Normal phase-liquid chromatography-tandem mass spectrometry with atmospheric pressure photoionization for the purity assessment of 17β-estradiol

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Abstract

A normal phase-liquid chromatography-hybrid tandem mass spectrometry (NP-LC-MS/MS) method utilizing atmospheric pressure photoionization (APPI) without dopant has been developed and implemented for the simultaneous determination of several estrogenic steroid hormones. The combination of both NP-LC and APPI-MS/MS tolerates the use of solvents that have the advantages of being self-doping for APPI and, at the same time, inhibit the in situ formation of estrogen dimers as frequently observed for conventional reversed phase (RP)-LC methods. The NP-LC-APPI-MS/MS method has been validated in-house, and its performance characteristics (linearity, repeatability, limits of detection, etc.) were assessed for use in the quantification of estrogens. Moreover, the method was used to characterize and determine the inherent related structure impurities in batches of β-estradiol, required for the establishment of reference measurement systems for clinical chemistry and laboratory medicine, which served as candidate reference material for an organic purity assessment interlaboratory study (CCQM-K55.a) organized by the International Bureau of Weights and Measures (BIPM) Chemistry Department and carried out within the framework of the Organic Analysis Working Group (OAWG) of the Consultative Committee for Amount of Substance—Metrology in Chemistry (CCQM).

Full-scale and enlarged overlaid SRM chromatograms of three transitions for ten estrogenic steroid hormones for the impurity quantification of a βE2 material

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Acknowledgments

The authors wish to acknowledge the National Metrology Institute of Japan (NMIJ) for providing the CCQM-K55.a (17β-estradiol) source material.

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Authors and Affiliations

  1. Département de Chimie, Bureau International des Poids et Mesures, Pavillon de Breteuil, 92312, Sèvres Cedex, France

    Ralf Dieter Josephs, Adeline Daireaux, Tiphaine Choteau, Steven Westwood & Robert Ian Wielgosz

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  1. Ralf Dieter Josephs
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  2. Adeline Daireaux
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  3. Tiphaine Choteau
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  4. Steven Westwood
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  5. Robert Ian Wielgosz
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Correspondence to Ralf Dieter Josephs.

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Published in the topical collection Reference Materials for Chemical Analysis with guest editors Hendrik Emons and Stephen A. Wise.

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Josephs, R.D., Daireaux, A., Choteau, T. et al. Normal phase-liquid chromatography-tandem mass spectrometry with atmospheric pressure photoionization for the purity assessment of 17β-estradiol. Anal Bioanal Chem 407, 3147–3157 (2015). https://doi.org/10.1007/s00216-014-8189-6

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  • DOI: https://doi.org/10.1007/s00216-014-8189-6

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