Forensic Biology & Its biological significance.pdf
Analysis of organic acids in e-vapor products by ion chromatography
1. Analysis of Organic Acids in E-Vapor Products
by Ion Chromatography
ZHU J.*; SNEAD E.; HAGERTY G.
ITG Brands, LLC, Greensboro, NC, USA
CORESTA SSPT2021
*Email: jeff.zhu@itgbrands.com
2021_ST22_ZhuJeff.pdf
SSPT2021
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Document
not
peer-reviewed
by
CORESTA
2. Introduction
• Organic acids (formic acid, acetic acid, propionic acid and lactic acid)
are of interest for e-vapor products testing, especially propionic acid
which is included in guidance from FDA-CTP1.
• Here we present a simple and low-cost method for the analysis of
these organic acids in E-vapor aerosols and e-liquids by ion
chromatography.
1) No derivatization needed – “shake and shoot”.
2) Use DI water as extraction solution and mobile phase (with KOH)
– no organic solvent required for the method.
1) Premarket Tobacco Product Applications for Electronic Nicotine Delivery Systems - Guidance for
Industry, FDA Center for Tobacco Products, June 2019.
2021_ST22_ZhuJeff.pdf
SSPT2021
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Document
not
peer-reviewed
by
CORESTA
3. Method – Instrument
IC Instruments: Thermo ICS 5000 or ICS 6000
Column: Dionex IonPac AS11-HC-4μm Analytical Column 2 x 250 mm
Column temperature: 30 °C
Flow rate: 0.35 mL/min
Mobile phase : KOH in DI water (Gradient see table below)
Time (min) KOH (mM) Curve
0 1.2 5
6 1.2 5
9.9 2.5 5
10 40 5
13.9 40 5
14 1.2 5
19 1.2 5
2021_ST22_ZhuJeff.pdf
SSPT2021
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Document
not
peer-reviewed
by
CORESTA
4. Method – Instrument
Autosampler temperature: set at 4 °C
Injection volume: 6 µL
Suppressor: ADRS600, 2 mm
Suppressor current: 35 mA
Detector cell temperature: 30 °C
Compartment temperature: 23 °C
Total runtime: 19 min
2021_ST22_ZhuJeff.pdf
SSPT2021
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Document
not
peer-reviewed
by
CORESTA
5. Method – Sample Preparation
Aerosol:
After aerosol collection*, transfer the glass fiber filter pad to 50 mL PP vial.
Add 36 mL of DI water into the vial and cap.
Shake on an orbital shaker for 30 minutes at 210 rpm.
Filter the solutions into PP autosampler vials through 0.2 µm PP filters.
E-Liquid:
Follows same process as aerosol using e-liquid instead of pad for extraction and
extraction at 300 rpm instead of 210 rpm.
*: 1) Cerulean SM 450 for ISO 20768, or Cerulean CETI-8 for either ISO 20768 or intense regime.
2) In-house trapping efficiency study shows >99% of analytes are collected in pads vs in impingers.
2021_ST22_ZhuJeff.pdf
SSPT2021
-
Document
not
peer-reviewed
by
CORESTA
6. Results – Calibration Curves on ICS 5000
- Range: 0.03 to 5 µg/mL
R2 = 0.99995
R2 = 0.99994
R2 = 0.99991
R2 = 0.99984
2021_ST22_ZhuJeff.pdf
SSPT2021
-
Document
not
peer-reviewed
by
CORESTA
7. Results – Signal to Noise Ratio
S/N at Low Standard levels
*: to quantitate the concentrations at LOQ spike levels during the validation
Instrument Standards S/N Lactic Acid Acetic Acid Propionic Acid Formic Acid
ICS 5000 Std 1S (0.03 µg/mL)* 30.7 73.8 44.0 92.5
Std 1 (0.05 µg/mL) 41.8 83.2 49.3 107.7
ICS 6000 Std 1S (0.03 µg/mL)* 50.3 65.6 44.9 122.1
Std 1 (0.05 µg/mL) 72.1 102.1 68.8 160.3
2021_ST22_ZhuJeff.pdf
SSPT2021
-
Document
not
peer-reviewed
by
CORESTA
12. Conclusions
• We have presented a simple and low-cost method for the analysis of organic
acids in E-vapor aerosols and e-liquids by ion chromatography.
• The method has been validated with good accuracies and is applicable to a
wide range of e-vapor products.
2021_ST22_ZhuJeff.pdf
SSPT2021
-
Document
not
peer-reviewed
by
CORESTA