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Introduction

The scientific community has been witness to the rise and fall and rise again of supercritical fluid chromatography (SFC) as a robust analytical tool. Due to advancements in instrumentation, such as back pressure regulators, we can begin to take SFC techniques out of the niche and place them amongst the ranks of GC and HPLC. In order to accomplish this, we need to establish a set of column parameters that will allow for the most efficient separations.Define column parameters for analytical scale SFC based on:

particle type
particle diameter
column dimensions

(Consider including a short section called “Key Aspects” here that summarizes your poster in a bullet point fashion)

ACT Program

Dr. Paige Wicker & Nazmee Parveen

Joisha Girme, Anna Romero, Ravi Ramkissoon

Acknowledgements

Introduction

Methods

Acknowledgements

Results/Expected Results

The Synthesis and Extraction of Endocrine Disrupting Steroids and The Kinetic Rates under Varying External Stressors

Destini Black, Aaliyah Devore, Phat Dinh, A. Paige Wicker, Nazmee Parveen, Frank W. Foss, Kevin A. Schug

Department of Chemistry and Biochemistry, The University of Texas at Arlington

Sample Preparation

Instrumentation

Conclusions/Future Work

MS Detection	LCMS-8040
Ionization Source	ESI (+)
Mode	MRM Precursor: 315.25 m/z Product: 97.00 m/z (CE=-24 eV) and 109.00 m/z (CE=-26 eV)
Nebulizing Gas Flow	2 L/min
DL Temperature	250° C
Heat Block Temperature	400° C
Drying Gas Flow	15 L/min

Background:

Reported side effect of birth control are nausea, dizziness, and psychological effects
Objective: To find a natural alternative for the intake of progesterone & to synthesize a degraded form of ethinyl estradiol.

Synthesis

Quantitative Study

Kinetic

3 step synthesis 6-⍺-hydroxy-ethinylestradiol

LC Parameters

Extraction and quantitation of progesterone from egg

Progesterone & 6-⍺-hydroxy-ethinylestradiol degradation under mimicked human conditions

Column	Restek Raptor C18 2.7 μm, 100 x 2.1 mm.
Mobile Phases	Solvent A: 5 mM ammonium acetate, 0.1% formic acid in water Solvent B: 5 mM ammonium acetate, 0.1% formic acid in methanol
Flow Rate	0.2 mL/min
Injection Volume	2 μL
Gradient	85% B → 100% B for 6 min, hold 4 min

Synthesis Schematics

NMR after every synthetic step
Expand the gradient to isolate progesterone peak
Determine LOD for quantitative study
Generate a standard addition calibration curve and study matrix effects
Test degradation in differing pH and temperature

References

1. Zia et al. Eur. J. Dent. 2019, 13(1), 124-128.

2. Kutztown University Mass Spectrometry. https://www.kutztown.edu/academics/colleges-and-departments/liberal-arts-and-sciences/departments/physical-sciences/chemistry-and-biochemistry/instrumentation/mass-spectrometry/lc-ms.html (accessed 2022-10-24).

3. Shimadzu-LCMS-8040 Liquid Chromatography. https://www.environmental-expert.com/downloads/shimadzu-model-lcms-8040-triple-quadrupole-liquid-chromatograph-mass-spectrometer-lc-ms-ms-brochure-813164 (accessed 2022-10-24).

4. Li et al. Food Sci. Nutr. 2019, 7(7), 2319-2326.

5. Weber et al. J F.Prakt.Chemie.1989, 331(2), 223-230.

6. York et al. Food Chem. 2020, 326(126939).

7. Shen et al. J. Chem. Eng. 2017, 327, 597-607.

8. Ekhato et al. Pub. Med. 2002, 67(3-4), 165-174.

9. Nejedly et al. Spinger. 2017, (24), 23196-23206.

Figure 6 (Expected Kinetic). Simple photodegradation of 17-alpha-ethinylestradiol in purified and seawater (25 °C). Purified water—black line; seawater (4 g L⁻¹)—blue line; seawater (32 g L⁻¹)—red line.⁹

Figure 1. Schematic presentation of a typical nuclear magnetic resonance spectrometer.¹

Figure 5 (Quantitative Study). External calibration curve of progesterone from 12.5-200 ppb

Weigh

Vortex

Centrifuge

Extract supernatants

Nitrogen stream

Syringe filtration

LC-MS/MS

Figure 4 (Quantitative Study). Chromatogram of 200 ppb progesterone

Area: 5,160,000±30,000

Figure 2. LC-MS/MS system with a triple quadrupole mass analyzer.^2,3