Calibration of analytical instrument
US-2024393301-A1 · Nov 28, 2024 · US
US9678087B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-9678087-B2 |
| Application number | US-201414533602-A |
| Country | US |
| Kind code | B2 |
| Filing date | Nov 5, 2014 |
| Priority date | Dec 13, 2007 |
| Publication date | Jun 13, 2017 |
| Grant date | Jun 13, 2017 |
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Provided are methods for determining the amount of estrone in a sample using mass spectrometry. The methods generally involve ionizing estrone in a sample and detecting and quantifying the amount of the ion to determine the amount of estrone in the sample.
Opening claim text (preview).
That which is claimed is: 1. A method for determining the amount of estrone in a human plasma or serum sample, said method comprising: (a) adding deuterated estrone to a human plasma or serum sample; (b) processing the sample by high performance liquid chromatography (HPLC); (c) ionizing estrone and deuterated estrone in said processed sample with electrospray ionization (ESI) in positive ion mode to produce one or more ions detectable by mass spectrometry; and (d) detecting the amount of the ions by tandem mass spectrometry; (e) comparing the amount of said one or more ions of estrone and said one or more ions of deuterated estrone to determine the amount of estrone in the sample; wherein said method has a limit of quantitation less than or equal to 500 pg/mL. 2. The method of claim 1 , wherein said estrone is derivatized prior to ionization. 3. The method of claim 1 , wherein said deuterated estrone is d 4 -estrone. 4. The method of claim 1 , wherein said deuterated estrone is 2,4,16,16-d 4 estrone. 5. The method of claim 1 , wherein said method further comprises subjecting estrone from said plasma or serum sample to an extraction. 6. The method of claim 1 , wherein said method has a limit of quantitation less than or equal to 20 pg/mL. 7. The method of claim 1 , wherein said method has a limit of detection less than or equal to 10 pg/mL. 8. A method for determining the amount of estrone in a human plasma or serum sample, said method comprising: (a) adding deuterated estrone to a human plasma or serum sample; (b) processing the sample by liquid chromatography; (c) ionizing estrone and deuterated estrone in said processed sample with electrospray ionization (ESI) in positive ion mode to produce one or more ions detectable by mass spectrometry; and (d) detecting the amount of the ions by tandem mass spectrometry; (e) comparing the amount of said one or more ions of estrone and said one or more ions of deuterated estrone to determine the amount of estrone in the sample; wherein said method has a limit of quantitation less than or equal to 500 pg/mL. 9. The method of claim 8 , wherein said estrone is derivatized prior to ionization. 10. The method of claim 8 , wherein said liquid chromatography comprises high turbulence liquid chromatography (HTLC). 11. The method of claim 8 , wherein said liquid chromatography comprises high performance liquid chromatography (HPLC). 12. The method of claim 8 , wherein said deuterated estrone is d 4 -estrone. 13. The method of claim 8 , wherein said deuterated estrone is 2,4,16,16-d 4 estrone. 14. The method of claim 8 , wherein said method further comprises subjecting estrone from said plasma or serum sample to an extraction. 15. The method of claim 8 , wherein said method has a limit of quantitation less than or equal to 20 pg/mL. 16. The method of claim 8 , wherein said method has a limit of detection less than or equal to 10 pg/mL. 17. A method for determining the amount of estrone in a human plasma or serum sample, said method comprising: (a) adding deuterated estrone to a human plasma or serum sample; (b) ionizing estrone and deuterated estrone in said processed sample with electrospray ionization (ESI) in positive ion mode to produce one or more ions detectable by mass spectrometry; and (c) detecting the amount of the ions by tandem mass spectrometry; (d) comparing the amount of said one or more ions of estrone and said one or more ions of deuterated estrone to determine the amount of estrone in the sample; wherein said method has a limit of quantitation less than or equal to 500 pg/mL. 18. The method of claim 17 , wherein said estrone is derivatized prior to ionization. 19. The method of claim 17 , wherein said deuterated estrone is d 4 -estrone. 20. The method of claim 17 , wherein said deuterated estrone is 2,4,16,16-d 4 estrone. 21. The method of claim 17 , wherein said method further comprises subjecting estrone from said plasma or serum sample to an extraction. 22. The method of claim 17 , wherein said method has a limit of quantitation less than or equal to 20 pg/mL. 23. The method of claim 17 , wherein said method has a limit of detection less than or equal to 10 pg/mL.
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