Name: Chantel Ubaezuonu Date: 05/02/2021 Group C
GCMS Analysis of Nicotine (Experiment 5)
Analysis of Vaping solution using GCMS along with an isotopically labelled standard.
Aim: The aim of this lab is to successfully analyze nicotine in e cigarettes using GCMS
Introduction:
In this experiment vaping solution using GCMS along with an isotopically labeled standard was successfully analyzed. The Vaping Industry has grown significantly throughout the years. Electronic cigarettes are relatively new battery powered devices that work by vaporizing a fluid containing nicotine. Vaping fluid is the fluid used in vaporizers to create a vapor. It comes in a variety nicotine levels including ones with zero nicotine options. It is made up of propylene glycol or vegetable gylcerin .There are over 50 million electronic cigarette users worldwide, mostly as an alternative to cigarettes. These e-cigarettes contain nicotine which is quite addictive and dangerous to humans. With increased use of EC’s, a large market for these products have shot up, there are numerous e-liquids available in multiple nicotine concentrations with approx. 7700 different flavors. There are e-cigs, e-hookahs and e-pipes.
In this experiment the GCMS is used. Gas chromatography-mass spectrometry (GC-MS) is a powerful method for the separation and identification of compounds based on differences in their chemical properties and is a particularly useful method for determining nicotine content in e-liquids. GC-MS can be used to study liquid, gaseous or solid samples. Analysis begins with the gas chromatograph, where the sample is effectively vaporized into the gas phase and separated into its various components using a capillary column coated with a stationary (liquid or solid) phase. The compounds are propelled by an inert ca
ier gas such as helium, hydrogen or nitrogen. As components of the mixture are separated, each compound elutes from the column at a different time based on its boiling point and polarity. The time of elution is refe
ed to as a compound's retention time. GC has the capacity to resolve complex mixtures or sample extracts containing hundreds of compounds. The SIM mode is used in this experiment. Selected Ion Monitoring (SIM) allows the mass spectrometer to detect specific compounds with very high sensitivity. In SIM mode, the instrument is set to gather data at masses of interest, instead of stepping the mass filter over a wide range of masses. Since the mass spectrometer collects data at only the masses of interest, it responds only to those compounds that possess the selected mass fragments. It gives more accurate and precise results
Fig 1 nicotine structure
Methods
No physical lab was ca
ied out due to covid 19 rules. This was an online lab.
Results
Nicotine Conc
Peak Area
ISTD
STD No
PPM (mg/L)
Counts
Peak area
1
10698
1625
2
15642
1011
3
20546
830
4
26207
751
5
43221
960
Nicotine
ISTD
Peak area
Peak area
36422
856
12741
958
Table 1.
Area ratio
Peak area ratio
10
6.583
20
15.47
30
24.75
40
34.89
50
45.02
Table 2.
Figure 2 cali
ation curve
Calculations
Calculation of volume required for standards
Concentration required / concentration given x final volume = volume required
0.2mg/mL / 1mg/mL x 5mL = 1 mL for standard one
0.4mg/mL / 1mg/mL x 5mL = 2 mL for standard two
0.6mg/mL / 1mg/mL x 5mL = 3 mL for standard three
0.8mg/mL / 1mg/mL x 5mL = 4 mL for standard fou
1mg/mL / 1mg/mL x 5mL = 5 mL for standard five
X axis = concentration of the standard / concentration of internal standard
1/0.1 = 10
2/0.1 = 20
3/0.1 = 30
4/0.1 = 40
5/0.1 = 50
Y axis = peak area of standard / peak area of internal standard
10698 / 1625 =6.583
15642 / 1011 = 15.47
20546 / 830 = 24.75
26207 / 751 = 34.89
43221 / 960 = 45.02
Area Ratio:
Peak A : 36422/856 = 42.55
Peak B: 12741/ 958 = 13.29
Y = 0.964x XXXXXXXXXX
Peak A = 42.55 = 0.964x XXXXXXXXXX
X = 47.86
47.86 x 0.1 = 4.786 mg / L
Peak B =13.29 = 0.964x XXXXXXXXXX
X = 17.51
17.51 x 0.1 = 1.751 mg/ L
Discussion
Maltol is an organic compound is used in confectionary. It appears as sugar but has a scent, which are like cooked fruits or caramel. Maltol helps to sweeten vaping liquid while adding a "candy taste" to the preparations of the e-cigarette providing a taste of cotton candy. It also helps to modify dry side and round flavoring. The use of Maltol is multiple, it is an indispensable additive to make a satisfying vaping liquid for electronic cigarette. Its chemical formula is C6H6O3. It has a molecular weight of XXXXXXXXXXg/mol
Acetic acid acidic gases and organic acid that is typically found in vinegar it has a very pungent smell and sour taste. In large doses it can be toxic to humans it is also found in photographic film and wood glue. It is found in cigarettes and is the cause of cancer. Carcinogens- chemicals known to cause cancer, including acetaldehyde and formaldehyde
As shown in Figure 2 a linear response was obtained for the five standards displaying good analytical skills and adherence to good laboratory practice also. The method was shown to be very linear and from the graph it gave an a r2 value of XXXXXXXXXXThey were analysed in the same manner of the standards and their individual peak areas were obtained in order to determine their concentrations of nicotine by the equation of the line. Finally, the GC methodology was revealed to be a powerful approach for accurate identification of volatile odour-active compounds in high-level complexity matrices through coupling traditional chromatographic analysis with human sensory perception. For this reason, the GC MS methodology was applied in the present study, allowing us to accurately identify, on a limited number of e-liquids, the odour-active compounds responsible for the overall flavour perceived or of specific flavour notesGC-MS proved to be a robust, repeatable, and sensitive method for determining the nicotine content of e-liquids based on measurements of accuracy and precision. The method used to quantify nicotine in vaping fluid was the selected ion monitoring modes of mass spectrometry (SIM) . The use of selected ion monitoring allows quick calculations of area ratios and shows the versatility of mass spectrometry, especially for more complex sample matrices.
Questions?
What is an isotopically labelled standard and why is it useful in mass spectrometry?
An isotopically labeled standard are said to be the most appropriate internal standard in mass spectrometry. this standard always compensates for variance in chemical derivatization, sample extraction and MS analysis
Why is the ion ratio of nicotine important in a QC lab?
The ion ratio is calculated as an intensity ratio of a less intense ion to that of a more intense ion. It is important for the use of the GCMS
In terms of the instrument set up what is the difference between the scan mode and the sim mode?
Scan or SIM mode can be used for GCMS analysis depending on the aim if the experiment.
Scan mode (qualitative analysis and quantitative analysis) is used for the identificatio of chemical components using a mass spectrum, quantitative analysis and determination of some parameter for SIM analysis .
Sim mode (quantitative analysis)
lower detection linits and can be obtained with the sim mode than the scan mode for qautitative analysis, because the sensitivity to hundred times bette
Conclusion:
Overall the experiment was successful. This approach of using gcms offers distinct advantages over previous methods, including analyte identification, ease of sample preparation and good reproducibility As electronic cigarettes explode in popularity, public attention is rapidly turning toward consumer safety. While research to date has focused primarily on the components of e-cigarette solutions, data presented here indicate a need for substantially more research into the chemical profile of vapor samples. The aim of the experiment was accomplished as the level of nicotine in a e-liquid sample was found, the results were obtained and analysis of the standards represented good laboratory practice for the group. Overall, the experiment was well conducted and successful.
References
Krüsemann, E.J.Z, Pennings, J.L.A., Cremers, J.W.J.M., Bakker, F., Boesveldt, S., Talhout, R. (2020) ‘GC–MS analysis of e-cigarette refill solutions: A comparison of flavoring composition between flavor categories’, Journal of Pharmaceutical and Biomedical Analysis, 188.
Fa
ell, G. (2018) ‘Spectroscopy’, INST-SC602: Instrumental 1, Letterkenny Institute of Technology, unpublished.
Paggano, T., Bida, R.M., Robinson, R.J. (2015) ‘Laboratory Activity for the Determination of Nicotine in Electronic Cigarette Liquids using Gas Chromatography-Mass Spectrometry’, J. Lab Chem Education, 3(3), 37-43.
Microsoft Word - Analytical practicals Manual
11
Experiment 5: Analysis of Vaping solution using GCMS along with
an isotopically labelled standard
Vaping is the inhaling of a vapor created by an electronic cigarette (e-cigarette) or
other vaping device. E-cigarettes are battery-powered smoking devices. They have
cartridges filled with a liquid that usually contains nicotine, flavourings, and
chemicals. The liquid is heated into a vapour, which the person inhales. E-Liquid
strength is almost always measured in milligrams (weight) per millilitre (volume);
expressed as mg/mL. Often the “per mL” (/mL) is dropped in conversation or
informal writing (and even on many labels). E-Liquid, comes in many varying
strengths depending largely on the manufacturer, sometimes even as high as 36 or
42mg/mL by can range from, 3, 6, 12, and 18 mg/mL, for example. In this experiment
you will.
1. Create a series of 5 standards from a nicotine stock of known concentration
2. Add the appropriate ISTD as indicated by the table below
3. Prepare the sample as indicated below
4. Analyse the vaping liquid itself
Your samples and standards are then analysed using an Agilent 5975 GCMS set to run
in SIM mode for the analysis of the standards and samples.
Sample/Standard preparation.
You are given a nicotine standard with a concentration of 10 PPM. Using the
automatic 1mL pipette provided, pipette the co
ect amount from the table below into
5 GC vials (provided) labelled STD 1 – 5 leave your sample vial empty for the
moment. Once this is complete, change the pipette tip and add the co
ect amount of
ISTD to all of your standards and samples. Change your pipette tip again and add the
co
ect amount of the sample to the sample vial. Finally change the tip again and add
the co
ect amount of TMP to