کد مقاله | کد نشریه | سال انتشار | مقاله انگلیسی | نسخه تمام متن |
---|---|---|---|---|
7610120 | 1493486 | 2016 | 34 صفحه PDF | دانلود رایگان |
عنوان انگلیسی مقاله ISI
A rapid method for the separation of vitamin D and its metabolites by ultra-high performance supercritical fluid chromatography-mass spectrometry
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کلمات کلیدی
موضوعات مرتبط
مهندسی و علوم پایه
شیمی
شیمی آنالیزی یا شیمی تجزیه
پیش نمایش صفحه اول مقاله
![عکس صفحه اول مقاله: A rapid method for the separation of vitamin D and its metabolites by ultra-high performance supercritical fluid chromatography-mass spectrometry A rapid method for the separation of vitamin D and its metabolites by ultra-high performance supercritical fluid chromatography-mass spectrometry](/preview/png/7610120.png)
چکیده انگلیسی
In this study, a new supercritical fluid chromatography-mass spectrometry (SFC-MS) method has been developed for the separation of nine vitamin D metabolites within less than eight minutes. This is the first study of analysis of vitamin D and its metabolites carried out by SFC-MS. Six columns of orthogonal selectivity were examined, and the best separation was obtained by using a 1-aminoanthracene (1-AA) column. The number and the position of hydroxyl groups in the structure of the studied compounds as well as the number of unsaturated bonds determine the physiochemical properties and, thus the separation of vitamin D metabolites that is achieved on this column. All D2 and the D3 forms were baseline separated with resolution values > 1.5. The effects of pressure, temperature, flow rate and different gradient modes were studied. Electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) were compared in positive mode, both by direct infusion and after SFC separation. The results showed that the sensitivity in APCI+ was higher than in ESI+ using direct infusion. In contrast, the sensitivity in APCI+ was 6-fold lower than in ESI+ after SFC separation. The SFC-MS method was validated between 10 and 500 ng/mL for all analytes with coefficient of determination (R2) â¥Â 0.999 for all calibration curves. The limits of detection (LOD) were found to range between 0.39 and 5.98 ng/mL for 24,25-dihydroxyvitamin D3 (24,25(OH)2D3) and 1-hydroxyvitamin D2 (1OHD2), respectively. To show its potential, the method was applied to human plasma samples from healthy individuals. Vitamin D3 (D3), 25-hydroxyvitamin D3 (25OHD3) and 24,25(OH)2D3 were determined in plasma samples and the concentrations were 6.6 ± 3.0 ng/mL, 23.8 ± 9.2 ng/mL and 5.4 ± 2.7 ng/mL, respectively.
ناشر
Database: Elsevier - ScienceDirect (ساینس دایرکت)
Journal: Journal of Chromatography A - Volume 1440, 1 April 2016, Pages 191-200
Journal: Journal of Chromatography A - Volume 1440, 1 April 2016, Pages 191-200
نویسندگان
Firas Jumaah, Sara Larsson, Sofia Essén, Larissa P. Cunico, Cecilia Holm, Charlotta Turner, Margareta Sandahl,