GCMS-QP2010 and SPME

with AOC 5000:

2,4,6 Trichloroanisole in cork
stoppers and wine
Standard and fast analysis

2,4,6 Trichloroanisole
in cork stoppers and wine

HS-SPME

GC-ECD EI-GCMS(SIM)



2,4,6 TCA




50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200 210 m/z
0.0
1.0
2.0
3.0
4.0
5.0
6.0
7.0
8.0
9.0
10.0
Inten. (x100)
195
197
210
212
167
169
97
109
74 62
107
145 83
49 132
143 53 201
160
71
OMe
Cl
Cl
Cl
2,4,6,TCA
C7H5CL3O
MW 210
CAS: 87-40-1
Wiley Library

2,4,6 TCA




1 ppb standard liquid injected
Splitless HPI 200 KPa 1 min

TRB 5 25 m, 0.25 mm, 0.25 m
40 C 2 min, 15 C/min 250C 10 min
He 49.2 cm/s constant
Scan 150 250 amu every 0.3 s

RT 10.06 min


Samples of 50 cork stoppers were placed in glass containers, filled with 2 L of
hydroalcoholic solution 12% v/v (soak solution).
The cork stoppers were maintained completely immersed in the soak solution,
during 24 hours at room temperature.
After this period, an aliquot of 10 ml was taken in a 20 ml vial, saturated with
NaCl (3g approximately). The instrumental analysis was performed using
SPME GCMS technique.
The instrumental conditions were as follows:
Column: 25m x 0,25mm, 0,25um film; 5% Diphenyl polydimethylsiloxane
Carrier gas: Helium
Injector: in splitless at 220C
Interface temperature: 280C
Fiber: 50/30 m DVB/PDMS (Carboxen possible),sampling headspace

Sample preparation


Internal standard:

Dissolve 5 mg of internal standard (2H5-2,4,6-TCA) in 1000 ml of ethanol
IS1
Dilute 8 ml of IS1 in 200 ml distilled water IS2 solution
Dilute 5 ml of IS2 in 500 ml distilled water IS3 solution

Analytes:

Dissolve 5 mg of each analyte (2,4,6-TCA; 2,3,5,6-TCA and PCA) in 1000ml
of ethanol SM1 solution.
Dilute 3 ml of SM1 in 500 ml distilled water SM2 solution
Dilute 2 ml of SM2 in 500 ml distilled water SM3 solution
From SM3, prepare standards in the range 0,5-50 ppt in 50 ml volumetric
flask. To each flask add 6 ml ethanol assuring 12% v/v alcoholic content.
From each standard, take 10ml in 20 ml vials (previously saturated with 3 g
NaCl), and add 200ul of IS3 solution (internal standard).


2,4,6 TCA




Standard SPME-GCMS:
HS-SPME Parameters: Fiber 50/30 m DVB/PDMS (Supelco)
(DVB/Carboxen)
Adsorption
Temp. 50 C
Time 30 min
Agitation 500 rms

Desorption
Inj Temp.: 220 C
Time 1 min

Inj Mode Splitless
Time 2 min
High Pressure Inj 200 kPa 2 min



Automatic SPME with AOC 5000




Agitator
X - Y - Z Robot
Wash Port
Liquid sample Tray
Headspace sample Tray
GCMS QP2010

AOC 5000
Rapid and easy change between modes just by....
syringe replacement
Gastight Headspace Syringe
+ Heating Block
SPME Fiber Holder
and different Fibers
Liquid Syringe Assy