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For quantification of sex hormones in serum, majority of the published methods included LLE for extraction of targets from serum matrix. Such results clearly demonstrated that CIPS extraction coupling LC-MS/MS analysis can provide robust quantification of sex hormones in wide concentration ranges. Enrichment factor was the ratio of target concentration in upper phase after CIPS to the original solution before adding water. Group III was serum samples in group II spiked with the same concentration of targets as group I.
It is worthwhile noting that the endo QC values from the two procedures are identical, indicating that the one-step procedure offers the same assay quality. By comparison, back-calculation used only the curve prepared using the two-step procedure while the curve prepared by the one-step procedure was used as QC. 1, the signal-to-noise of the LLOQ from the one-step procedure is slightly higher than that for the two-step procedure. Data in Table 2 indicate that there is no difference for testo extracted by either procedure, indicating that neither procedure introduces detectable interference into the testo peak.
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In this study, based also on literature data, the effectiveness of extraction procedures of steroid hormones from urine samples was assessed. Moreover, the goal of the study was also to demonstrate the application of the elaborated method for routine doping control and the quantification of steroid hormones in human urine samples. Therefore, the aim of this study was to develop electrophoretic methods for the identification and determination of steroid hormones in urine samples of volunteers and amateur weight-lifters by the micellar electrokinetic capillary chromatography (MEKC) technique. We assessed precision of the method as intra-day and inter-day variations from repeated analysis of fortified human urine and serum samples.
Analyst software v1.7.2 (ABSciex, Framingham, MA, USA) was used for data analysis. The quantification of target analytes was performed on an ABSciex 5500+ Q-trap mass spectrometer (Framingham, MA, USA) coupled to an ExionLC HPLC (SCIEX, Redwood City, CA, USA). Estrogens were then selectively derivatized by the addition of 125 µL of sodium bicarbonate buffer (0.1 M; pH 9.0) and 125 µL of dansyl chloride (1 mg/mL in acetone), vortexed vigorously (~30 s), and the sample tubes were immediately kept at 60 °C (on a hot plate) for 5 min. After gentle mixing, the samples were incubated overnight (~15 h) at 37 °C by shaking at 100 rpm (Jeio Tech Co., Seoul, South Korea). Bond Elut C18 (60 mg/3 mL), Bond Elut Plexa (60 mg/3 mL), and Bond Elut NEXUS (60 mg/3 mL) solid phase extraction (SPE) cartridges were obtained from Agilent Technologies (Santa Clara, CA, USA).
After incubation (10 min) at 65°C, the mixture was transferred for LC-MS/MS analysis. The resulting solution was centrifuged (10,000 g) at 4°C for 2 min and stored at −30°C for 10 min to conduct CIPS. These samples were obtained from the excess samples after routine detection services. We expect that the new method can be a promising alternative for daily sex hormone analysis in routine clinical laboratories.
For acid and alkali hydrolysis samples were treated with 10 ml of 1 M HCl and 1 M NaOH and then sonicate for 30 min and then stayed for 1.5 hours. During performing robustness test standard stock solution at concentration of 40 ppm Testosterone Undecanoate was used and it was found that all the criteria for system suitability was satisfactory. System suitability was determined by injecting five replicate standard solution from same vial before analyze test sample each day. It was prepared by using 5 concentrations with three replicates by diluting stock solution to the concentrations of 20, 32, 40, 48 and 60 ppm. Many analytical methods has been proposed for quantitative determination of testosterone undecanoate such as UV method 24,25, gas chromatography-mass spectroscopy 21,26,27, LCMS/ MS method 28-31, nuclear magnetic resonance , LC-QTOF/ MS .
Few earlier studies employed lengthy chromatographic separation time to isolate and resolve individual analytes 5,19. LOD and LOQ of target analytes in urine were calculated as 3 and 10 times the standard deviation (SD), respectively. The inter-day CV was measured by repeated injection of fortified samples on three different days.