Analysis of steroids in urine by gas chromatography-capillary photoionization-tandem mass spectrometry
Copyright © 2019 Elsevier B.V. All rights reserved..
A new heated capillary photoionization (CPI) ion source design was developed to photoionize analytes inside a transfer capillary between a gas chromatograph (GC) and a mass spectrometer (MS). The CPI setup included a wide, oval-shaped vacuum-ultraviolet (VUV) transparent magnesium fluoride (MgF2) window to maximize photoionization efficiency and thus sensitivity. The source contained a nitrogen housing around the ionization chamber inlet to avoid undesirable hydrolysis and oxidation reactions with ambient air and to maximize the proportion of formed molecular radical cations of analytes. The feasibility of the ion source was studied by analyzing 18 endogenous steroids in urine as their trimethylsilyl (TMS) derivatives with gas chromatography-tandem mass spectrometry (GC-MS/MS). The method was validated and applied to human urine samples. To our best knowledge, this is the first time that a capillary photoionization ion source has been applied for quantitative analysis of biological samples. The GC-CPI-MS/MS method showed good chromatographic resolution (peak half-widths between 3.1 to 5.3 s), acceptable linearity (coefficient of determination between 0.981 to 0.996), and repeatability (relative standard deviation (RSD%) between 5 to 18%). Limits of detection (LOD) were between 2 to 100 pg mL-1 and limits of quantitation (LOQ) were between 0.05 to 2 ng mL-1. In total, 15 steroids were quantified either as a free steroid or glucuronide conjugate from the urine of volunteers. The new CPI source design showed excellent sensitivity for analysis of steroids in complex biological samples.
| Medienart: |
E-Artikel |
|---|
| Erscheinungsjahr: |
2019 |
|---|---|
| Erschienen: |
2019 |
| Enthalten in: |
Zur Gesamtaufnahme - volume:1598 |
|---|---|
| Enthalten in: |
Journal of chromatography. A - 1598(2019) vom: 02. Aug., Seite 175-182 |
| Sprache: |
Englisch |
|---|
| Beteiligte Personen: |
Pöhö, Päivi [VerfasserIn] |
|---|
| Links: |
|---|
| Themen: |
Capillary photoionization |
|---|
| Anmerkungen: |
Date Completed 03.07.2019 Date Revised 10.12.2019 published: Print-Electronic Citation Status MEDLINE |
|---|
| doi: |
10.1016/j.chroma.2019.03.061 |
|---|
| funding: |
|
|---|---|
| Förderinstitution / Projekttitel: |
|
| PPN (Katalog-ID): |
NLM296241474 |
|---|
| LEADER | 01000naa a22002652 4500 | ||
|---|---|---|---|
| 001 | NLM296241474 | ||
| 003 | DE-627 | ||
| 005 | 20231225085417.0 | ||
| 007 | cr uuu---uuuuu | ||
| 008 | 231225s2019 xx |||||o 00| ||eng c | ||
| 024 | 7 | |a 10.1016/j.chroma.2019.03.061 |2 doi | |
| 028 | 5 | 2 | |a pubmed24n0987.xml |
| 035 | |a (DE-627)NLM296241474 | ||
| 035 | |a (NLM)31003716 | ||
| 035 | |a (PII)S0021-9673(19)30329-2 | ||
| 040 | |a DE-627 |b ger |c DE-627 |e rakwb | ||
| 041 | |a eng | ||
| 100 | 1 | |a Pöhö, Päivi |e verfasserin |4 aut | |
| 245 | 1 | 0 | |a Analysis of steroids in urine by gas chromatography-capillary photoionization-tandem mass spectrometry |
| 264 | 1 | |c 2019 | |
| 336 | |a Text |b txt |2 rdacontent | ||
| 337 | |a ƒaComputermedien |b c |2 rdamedia | ||
| 338 | |a ƒa Online-Ressource |b cr |2 rdacarrier | ||
| 500 | |a Date Completed 03.07.2019 | ||
| 500 | |a Date Revised 10.12.2019 | ||
| 500 | |a published: Print-Electronic | ||
| 500 | |a Citation Status MEDLINE | ||
| 520 | |a Copyright © 2019 Elsevier B.V. All rights reserved. | ||
| 520 | |a A new heated capillary photoionization (CPI) ion source design was developed to photoionize analytes inside a transfer capillary between a gas chromatograph (GC) and a mass spectrometer (MS). The CPI setup included a wide, oval-shaped vacuum-ultraviolet (VUV) transparent magnesium fluoride (MgF2) window to maximize photoionization efficiency and thus sensitivity. The source contained a nitrogen housing around the ionization chamber inlet to avoid undesirable hydrolysis and oxidation reactions with ambient air and to maximize the proportion of formed molecular radical cations of analytes. The feasibility of the ion source was studied by analyzing 18 endogenous steroids in urine as their trimethylsilyl (TMS) derivatives with gas chromatography-tandem mass spectrometry (GC-MS/MS). The method was validated and applied to human urine samples. To our best knowledge, this is the first time that a capillary photoionization ion source has been applied for quantitative analysis of biological samples. The GC-CPI-MS/MS method showed good chromatographic resolution (peak half-widths between 3.1 to 5.3 s), acceptable linearity (coefficient of determination between 0.981 to 0.996), and repeatability (relative standard deviation (RSD%) between 5 to 18%). Limits of detection (LOD) were between 2 to 100 pg mL-1 and limits of quantitation (LOQ) were between 0.05 to 2 ng mL-1. In total, 15 steroids were quantified either as a free steroid or glucuronide conjugate from the urine of volunteers. The new CPI source design showed excellent sensitivity for analysis of steroids in complex biological samples | ||
| 650 | 4 | |a Journal Article | |
| 650 | 4 | |a Validation Study | |
| 650 | 4 | |a Capillary photoionization | |
| 650 | 4 | |a Dopant-assisted photoionization | |
| 650 | 4 | |a Gas chromatography | |
| 650 | 4 | |a Steroid | |
| 650 | 4 | |a Tandem mass spectrometry | |
| 650 | 4 | |a Urine | |
| 650 | 7 | |a Steroids |2 NLM | |
| 700 | 1 | |a Scholz, Karen |e verfasserin |4 aut | |
| 700 | 1 | |a Kärkkäinen, Niina |e verfasserin |4 aut | |
| 700 | 1 | |a Haapala, Markus |e verfasserin |4 aut | |
| 700 | 1 | |a Räikkönen, Heikki |e verfasserin |4 aut | |
| 700 | 1 | |a Kostiainen, Risto |e verfasserin |4 aut | |
| 700 | 1 | |a Vaikkinen, Anu |e verfasserin |4 aut | |
| 773 | 0 | 8 | |i Enthalten in |t Journal of chromatography. A |d 1993 |g 1598(2019) vom: 02. Aug., Seite 175-182 |w (DE-627)NLM074731416 |x 1873-3778 |7 nnns |
| 773 | 1 | 8 | |g volume:1598 |g year:2019 |g day:02 |g month:08 |g pages:175-182 |
| 856 | 4 | 0 | |u http://dx.doi.org/10.1016/j.chroma.2019.03.061 |3 Volltext |
| 912 | |a GBV_USEFLAG_A | ||
| 912 | |a GBV_NLM | ||
| 951 | |a AR | ||
| 952 | |d 1598 |j 2019 |b 02 |c 08 |h 175-182 | ||