Presentation is loading. Please wait.

Presentation is loading. Please wait.

Analysis of Caffeine in Coffee Kate Penrod, Nikki DeLuca, Christina Robinson, and Jess Bases.

Similar presentations


Presentation on theme: "Analysis of Caffeine in Coffee Kate Penrod, Nikki DeLuca, Christina Robinson, and Jess Bases."— Presentation transcript:

1 Analysis of Caffeine in Coffee Kate Penrod, Nikki DeLuca, Christina Robinson, and Jess Bases

2 Purpose Quantify caffeine in brewed coffee – Varying strengths Extract caffeine from grounds Maxwell House: Regular and Decaf.

3 Background Caffeine in food/drink CNS stimulant Schedule V drug High levels – Restlessness – Irritability – Headaches – Heart complications

4 Methods HPLC – Liquid Separation – Liquid IR – Solid and liquid SFE – Solid UV/Vis – Disabled

5 HPLC Hypothesis Samples – 10-50ppm caffeine standards – Strong caffeinated/decaffeinated – Regular caffeinated/decaffeinated – Weak caffeinated/decaffeinated Dilution of coffee samples

6

7 SampleConc [ppm]Retention TimeArea Standard Standard Standard Standard Standard Weak DC 1: Reg DC 1: Str DC 1: Weak C 1: Reg C 1: Str C 1:

8 Organic Separation Sample Preparation (Dr. Peterman’s Coffeemaker) – Regular Caffeinated/ Decaffeinated 1 Tbsp. grounds, ¾ cup water – Strong Caffeinated/ Decaffeinated 3/2 Tbsp. grounds, ¾ cup water – Weak Caffeinated/ Decaffeinated ½ Tbsp. grounds, ¾ cup water

9 Organic Separation First Method – Adapted from Dr. Halligan’s Organic I Lab Manual – Extraction of Caffeine using Dichloromethane – Large emulsion layer, not a clear separation

10 Organic Separation Revised Method – Added Na 2 CO 3 which increased caffeine’s solubility in aqueous layer – Separation layer more pronounced – Dried with Anhydrous MgSO 4 – Vacuum under reduced pressure

11 Mass Quantification AppearanceMass of Product Regular CaffeinatedYellow/brown liquid0.2753g Weak CaffeinatedLight brown liquid0.2731g Strong CaffeinatedYellow/ brown solid, black spots g Regular DecaffeinatedYellow/brown liquid g Weak DecaffeinatedLight brown liquid0.2001g Strong DecaffeinatedYellow/ brown liquid g

12 Extracted Caffeine IR Characterization Substituted Alkene

13 Extracted Caffeine IR Characterization Strong Decaff Regular Decaff Weak Decaff C = N C = O O – H stretch C = N C = O Substituted Alkene C = O C = N O – H stretch CH3 C - N Substituted Alkene

14 Extracted Caffeine IR Characterization Strong Caffeinated Regular Caffeinated C = O C = N O – H stretch CH3 C - N Substituted Alkene C = O C = N O – H stretch CH3 C - N Substituted Alkene C - N CH3 C = N O – H stretch Weak Caffeinated

15 The Devil’s Instrument a.k.a. SFE

16 4 Samples – “Pure” coffee grounds – Post brewing coffee grounds 1 gram of each sample 10 minute runs End mass indications IR results

17 SFE Data SamplePercent Yield Pure Caffeinated5.186 % Pure Decaf % Brewed Caffeinated1.185 % Brewed Decaf %

18 SFE Extraction IR Analysis

19 UV/Vis Attempted to use the DRA-600 – Solid Analysis Missing part! Call EVERYONE – Manufacturer – Distributor – Delivery Guy Piece was backordered until May 20 th Put on hold INDEFINITELY.

20 Sources of Error Organic Method – Impure caffeine for mass quanitification – Transfer between different glassware – Incomplete drying in extraction (O-H stretch peak) HPLC – Day 1: Low pressure, purge lines – Day 2: Invalid date/time error, inconsistent – Day 3: Consistent results, ran all samples

21 Sources of Error (Part 2) SFE – Leaks in the line – Issues with the amount of sample – Needed constant supervision UV/Vis – Missing part – Phone tag – Wasted 2 whole lab periods

22 Sources of Error (Part 3) Jerry Sainsbury – Sales Representative Thermo Fisher Scientific

23 Conclusions HPLC: Strong decaf. was comparable to weak caf. Weak and regular brews – 4:1 caf. vs. decaf. Strong brew – 5:2 caf. vs. decaf. Organic Method: Qualitative data Erroneous quantitative data Masses very similar SFE: Low percent yields Higher yield from decaf Did not extract pure caffeine May be caffeine plus side products If UV/Vis hadn’t been in the initial method, further research would have been conducted

24 Further Research Organic Method – Develop a new or revised method to extract pure caffeine in its solid form as was done in Dr. Halligan’s Organic I Lab IR – Analyze liquid only – Create calibration curve HPLC – Compare different coffee makers and brands

25 Further Research (Part 2) SFE – Brew remaining grounds, analyze with HPLC – Determine other components of extracted grounds UV/Vis – Obtain calibration disc and sample holder – Develop SOP for DRA-600


Download ppt "Analysis of Caffeine in Coffee Kate Penrod, Nikki DeLuca, Christina Robinson, and Jess Bases."

Similar presentations


Ads by Google