Normal phase-liquid chromatography-tandem mass spectrometry with atmospheric pressure photoionization for the purity assessment of 17β-estradiol
- 283 Downloads
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).
KeywordsEstradiol Estrogen Purity Normal phase Photoionization LC-MS/MS
The authors wish to acknowledge the National Metrology Institute of Japan (NMIJ) for providing the CCQM-K55.a (17β-estradiol) source material.
- 2.Westwood S, Josephs RD, Daireaux A, Wielgosz RI, Davies S, Wang H, Rodrigues J, Wollinger W, Windust A, Kang M, Fuhai S, Philipp R, Kuhlich P, Wong S-K, Shimizu Y, Perez M, Avila M, Fernandes-Whaley M, Prevoo D, de Vos BJ, Visser R, Archer M, LeGoff T, Wood S, Bearden D, Bedner M, Boroujerdi A, Duewer D, Hancock D, Lang B, Porter B, Schantz M, Sieber J, White E, Wise SA (2012) Metrologia 49: Tech Suppl 08009Google Scholar
- 6.Okayasu Y, Komori K, Yasojima M, Suzuki Y (2005) In: Occurrence and treatment of emerging contaminants. Japanese Water Environment Federation Report, Japan, 291–297Google Scholar
- 8.Loeffler D, Ramil M, Ternes T, Suter M, Schoeneberger R, Aerni H-R, Koenig S, Besa A, Schreiber A (2006) Application note: estrogens. Applied Biosystems, Foster CityGoogle Scholar
- 9.Borton C, Ghobarah H, Olson L (2007) Application note: endocrine disrupting compounds. Applied Biosystems, Foster CityGoogle Scholar
- 14.OSHA Analytical Methods Index. Estradiol, estriol, estrone, 17-α-methyltestosterone progesterone, testosterone PV2001 (2001) US Dept. of Labor, Occupational Safety & Health Administration (OSHA), Salt Lake CityGoogle Scholar
- 15.Estradiol (2005) United States Pharmacopeia Official Monograph, US Pharmacopeial Convention, Rockville (MD), USP28, 772Google Scholar
- 26.Guo T, Chan M, Soldin S (2004) J Arch Pathol Lab Med 128:469–475Google Scholar
- 27.Miller C (2002) Application note: MSn analysis with fast polarity switching in the Agilent 1100 Series LC/MSD Trap SL. Agilent, Palo AltoGoogle Scholar
- 33.Analyze additional compound classes with the photospray atmospheric pressure photoionization source (2002) Product Bulletin LC-MS: Applied Biosystems, Foster CityGoogle Scholar