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A GC-FID system, Nexis GC-2060 (Shimadzu Corporation) was
employed in this work. The details of the system and analytical
conditions for this analysis method are shown in Table 1.
Fig. 1 Nexis GC-2060 with AOC-30i
Instrumentation and Analysis Conditions
The analysis of volatile substances and methanol in spirit drinks is
essential for regulatory compliance, quality control and
verification of product authenticity. Commission Regulation (EC)
No 2870/2000 establishes Community reference methods to
ensure harmonized results during official controls and in disputes;
gas chromatography with flame ionization detection (GC-FID) is
the specified reference technique for quantifying key volatile
congeners (aldehydes, higher alcohols, ethyl acetate) and
methanol.
1
This application note describes a GC-FID method for
these analytes on a Shimadzu Nexis GC-2060, implemented to
comply with the Regulation’s requirements and suitable for
routine and official-control testing across a range of spirit drink
categories.
This application note also evaluates Shimadzu Multi-Mode
Injection Unit (MMI) operated in split/splitless mode to verify its
performance to meet the requirements of the method.
Introduction
Nexis GC-2060 was validated for Commission Regulation (EC) No 2870/2000 for the official control of spirit drinks.
Nexis GC-2060 provides excellent separation, high linearity, and low RSDs for reliable routine throughput.
The Multi-Mode Injection Unit (MMI) demonstrated excellent performance to meet EC 2870/2000 criteria and significantly
reduces maintenance-related downtime.
The Analysis of Volatile Substances and Methanol
in Spirit Drinks Using Nexis GC-2060
Elvi Horiyanto
1
, Chun Kiang Chua
1
, Cynthia Lahey
1
, Chisato Kanamori
2
, Sixu Li
2
Gas Chromatograph Nexis GC-2060
1 Shimadzu Asia Pacific 2 Shimadzu Corporation
Standards Preparation
Table 2 shows the list of congeners and internal standard
analyzed in this work. Standard solutions A, B, C, D and E (to be
used as or for the preparation of calibration solutions, checking
resolution, QC Standard and internal standard spiking) were
prepared in close accordance with EC 2870/2000.
1
All reagents
were of analytical grade (purity ≥ 99 %), and ultrapure water
was used throughout. A 40 % (v/v) ethanol solution was
prepared by diluting absolute ethanol with water and served as
the solvent for all standard solutions. During preparation, the
mass of each component was recorded to ensure accurate
quantification of unknown samples.
Calibration solutions were prepared by combining appropriate
volumes of Solutions A and B to obtain final concentrations of
30, 150, 300, and 600 µL/L, with internal standard concentration
of 300 µL/L. The concentrations were subsequently recalculated
to µg/g for construction of the internal standard calibration
curve.
QC Standard was prepared by combining 9:1 volume ratio of
Solution D and E, resulting in a final concentration of
270 µL/L for each congener, with internal standard
concentration of 300 µL/L.
Standards and Sample Preparation
System Configurations
GC system Nexis GC-2060
Injection Port Multi-Mode Injection Unit (MMI)
Auto sampler AOC-30i
Column
SH-BAC Plus 1; 30 m x 0.32 mm x 1.80 µm
(P/N: 227-36260-01),
SH-502.2; 30 m x 0.25 mm x 1.40 µm
(P/N: 227-36341-04)
Both columns are connected in series.
AOC-30i Parameters
Sample Volume 0.5 μL
Gas Chromatograph Parameters
Injection Mode Split mode (Split Ratio: 20)
Carrier Gas Nitrogen
Flow Control Mode Linear velocity (25 cm/s)
Column Temperature
Program
60 ˚C (5 min)
→ 10 ˚C/min to 80 ˚C (18 min)
→ 30 ˚C/min to 200 ˚C (9 min)
FID Parameter
Detector Temperature 240 ˚C
Table 1. System Configurations and Analysis Conditions
ID # Compound Name
1 Methanol
2 Acetaldehyde
3 Propan-1-ol
4 Butan-2-ol
5 2-Methylpropan-1-ol
6 Ethyl acetate
7 Butan-1-ol
8 Pentan-3-ol (IS)
9 Acetal
10 3-Methylbutan-1-ol
11 2-Methylbutan-1-ol
Table 2. List of Congeners and Internal Standard (IS) Analyzed
Sample Preparation
For sample preparation, a measured volume of the spirit drink
sample was transferred into a sealed vessel, followed by the
addition of a fixed volume of Solution E. The mixture was
homogenised by inversion and, if necessary, diluted with 40 %
(v/v) ethanol to ensure analyte concentrations fell within the
calibration range. Prepared samples should be analysed
immediately to minimise the loss of volatile components.
Results and Calculation
Separation & Response Factor
Chromatographic separation under the GC conditions produced
clear and well-resolved peaks for all target analytes.
MMI enables rapid cooling, reducing the temperature from
230˚C to 70˚C in 7 minutes, compared with 32.2 minutes for
conventional SPL in this system. With the compressed air
cooling option, MMI can reduce the cooling time further to just
2.4 minutes. Although cooling time may vary depending on the
installation environment and air supply pressure, MMI still
significantly shortens maintenance downtime compared with
conventional SPL.
