Purity assignment of 17β-estradiol by mass balance method

다국어 초록 (Multilingual Abstract)

In general, quantitative chemical analysis in various areas including food, the environment, in vitro diagnostics, etc., requires traceability in order to increase the reliability of the measurements. Measurement traceability is a property of an unbroken chain of comparisons relating an instrument's measurements to SI units. Purity analysis is the first process for establishing traceability to SI units in chemical measurements. The purpose of this study is to develop and validate a method of purity assignment for establishing the traceability of 17β-estradiol measurements in an in vitro diagnostics field. The establishment of this method is very important as it can be applied to the development of CRM and to the analysis of the purity of other hormones. The method of assignment of the purity of 17β-estradiol was developed using the mass balance method and was validated through participation in an International comparison. In the mass balance method, impurities are categorized into four classes as follows: total related structure impurities, water, residual organic solvents, and nonvolatiles/inorganics. In this study, total related structure impurities were characterized by a gas chromatography-flame ionization detector (GC-FID) and a high-performance liquid chromatography-ultraviolet (HPLC-UV) detector, water content was determined by a Karl-Fisher coulometer, and total residual solvents and nonvolatiles/inorganics were checked simultaneously by thermogravimetric analysis (TGA). The purity of the 17β- estradiol was 985.6 mg/g and the expanded uncertainty was 2.1 mg/g at 95% confidence. The developed method can be applied to the development of certified reference materials, which play a critical role in traceability.

참고문헌 (Reference)

1 S. Westwood, 48 (48): 08013-, 2011

2 C. H. Wu, 43 (43): 436-445, 1976

3 R. Södergård, 16 (16): 801-810, 1982

4 S. Westwood, 49 (49): 08014-, 2012

5 S. Westwood, 49 (49): 08009-, 2012

6 R. Stricker, 44 (44): 883-887, 2006

7 S. Westwood, 85 : 3118-, 2013

8 S. Westwood, 46 (46): 08019-, 2009

9 J. F. Strauss, "Yen and Jaffe's Reproductive Endocrinology: Physiology, Pathophysiology, and Clinical Management" Elsevier Health Sciences 807-, 2009

10 J. B. Becker, "Sex Differences in the Brain:From Genes to Behavior" Oxford University Press 64-, 2007

11 이화심, "Method Development for Purity Assignment of l-Valine by a Mass Balance Method" 대한화학회 37 (37): 418-421, 2016

12 JCGM, "International Vocabulary of Metrology−Basic and General Concepts and Terms"

13 "ISO/IEC 17025"

14 "ISO 17511"

15 JCGM, "Evaluation of measurement data—guide to the expression of uncertainty in measurement"

16 "European Council Directive 98/79/EC"

17 R. F. Dons, "Endocrine and Metabolic Testing Manual" CRC Press 8-, 1994

18 I. D. Hay, "Clinical Endocrine Oncology" John Wiley & Sons 623-, 2009