LAAN-A-LM-E050
Liquid Chromatography Mass Spectrometry
No.C79
Analysis of Polymer Additives Using the LCMS-8030 Triple Quadrupole LC/MS/MS
Antioxidants, ultraviolet absorbers, flame retardants
and other polymer additives are indispensable for
improving the characteristics and functionality of
polymers. Understanding the types and quantities of
these additives to be used is extremely important to
effectively control the manufacturing process of the
polymers.
Below is an example of quantitative analysis of 14
types of polymer additives using MRM (Multiple
Reaction Monitoring) and the LCMS-8030 triple
quadrupole mass spectrometer.
n MRM Analysis with the LCMS-8030
Conducting MRM measurement with a triple quadrupole
mass spectrometer makes it possible to obtain
molecular structure information while simultaneously
performing quantitative analysis. Fig. 1 shows the
chromatograms of 14 polymer additives. Two additives
were analyzed in positive mode, and 12 were
analyzed in negative mode. Fig. 2 shows the calibration
curves of each of the constituents. Excellent linearity
was obtained for every compound tested.
(×10,000,000)
1.25
Irganox 245
585.30>367.20(-)
Irganox 1098
635.45>417.50(-)
Irganox MD 1024
1.00
Tinuvin P
226.10>107.10(+)
Cyanox 2246
0.75
339.15>163.20(-)
Cyanox425
367.25>177.20(-)
Irganox 1035
Irgafos 168 oxide
0.50
Tinuvin 120
Irganox 1010
2.5
3.0
3.5
4.0
4.5
5.0
5.5
6.0
6.5
663.50>57.15(+)
437.25>205.25(-)
350.25>319.85(-)
Irganox 1330
773.55>773.55(-)
Irganox 1076
529.45>41.15(-)
Irganox 565
0.00
641.35>83.20(-)
1175.70>1175.70(-)
Tinuvin 328
0.25
551.35>333.40(-)
587.35>58.10(-)
7.0 min
Fig. 1 Chromatograms of 14 Polymer Additives
Irganox 245
3.0
Irganox MD 1024
面積(×100,000)
1-500 ppb
2.5
2.25
1.00
R^2=0.995
0
100
200
300
400
濃度
0.00
Cyanox 425
500
750
濃度
7.0
5.0
R^2=0.996
0
100
200
300
400
5-500 ppb
2.0
0.5
R^2=0.997
0.0
25.0
50.0
75.0
濃度
0.0
0.0
Tinuvin 328
25.0
50.0
75.0
濃度
500-10000 ppb
1.0
0
2500
5000
7500
濃度
300
400
濃度
6.0
0
2500
5000
R^2=0.998
7500
濃度
0.00
0.0
25.0
50.0
75.0
濃度
Irganox 1076
1-1000 ppb
3.0
1.5
1.0
100
200
300
400
濃度
0.5
0.0
75.0
濃度
0.1-100 ppb
2.0
R^2=0.997
2.5
0
50.0
3.0
3.5
R^2=0.996
25.0
4.0
0.25
0.00
0.0
5.0
面積(×100,000)
0.5-500 ppb
0.25
0.5
0.0
200
0.50
1.5
R^2=0.999
0.01-100 ppb
2.0
2.0
0.50
100
0.75
2.5
0.75
0
0.0
Irganox 1010
0.50
R^2=0.996
R^2=0.997
0.5
面積(×10,000)
0.75
1.00
3.0
濃度
1.00
面積(×1,000,000)
0.5-10000 ppb
3.5
750
Tinuvin 120
Irganox 565
面積(×1,000,000)
4.0
1.00
0.25
0.0
500
1.25
1.0
Irganox 1330
面積(×100,000)
1.25
R^2=0.998
1.0
250
面積(×1,000,000)
1.50
2.0
3.0
1.0
R^2=0.999
1.75
3.0
4.0
1.5
0
面積(×10,000)
4.0
5.0
1.0
2.0
0.5
濃度
6.0
1.5
2.5
1.0
Irgafos 168 oxide
0.5-100 ppb
8.0
2.0
0.00
250
面積(×10,000)
0.01-100 ppb
2.5
0
0.00
0.01-100 ppb
3.0
1.5
0.25
Irganox 1035
面積(×1,000,000)
3.0
R^2=0.997
0.25
3.5
2.0
0.50
0.50
Cyanox 2246
面積(×1,000,000)
1-1000 ppb
2.5
0.75
0.5
0.0
5-500 ppb
0.75
1.25
1.0
Tinuvin P
面積(×100,000)
面積(×100,000)
1.00
1.50
1.5
0.0
1-1000 ppb
1.75
2.0
Irganox 1098
面積(×100,000)
2.00
R^2=0.999
0
250
500
Fig. 2 Calibration Curves of 14 Polymer Additives
750
濃度
1.0
0.0
R^2=0.997
0.0
25.0
50.0
75.0
濃度
No.C79
n Analysis of Unknown Polymer Additives Using the LCMS-8030
Quantitative analysis was conducted for the polymer
additives in a food wrapping material and food
container. THF (1 mL) was added to a pulverized
sample (0.1 g), and this was sonicated for 1 minute.
The supernatant was collected, 1 mL of 5 mM
ammonium acetate was added, and the final mixture
was filtered (0.45 μm.)
Fig. 3 shows the MS chromatograms and the MRM
Food Wrapping Material
(×10,000)
Food Container
(×100,000)
4.0
7.0
3.5
6.0
3.0
5.0
2.5
4.0
2.0
3.0
1.5
2.0
1.0
1.0
0.5
0.0
0.0
3.5
4.0
4.5
5.0
5.5
6.0
6.5
7.0 min
2.5
(×1,000)
4.859
2.0
1.5
4.0
4.5
49.7 ng/g
0.5
0.5
4.7
4.8
4.9
0.6
14.3 μg/g
6.5
7.0 min
(×1,000)
48.7 ng/g
0.4
0.2
3.1
3.2
3.3
3.4
Irganox 245
Fig. 3 Chromatograms of Polymer Additives Detected in the Analysis
(Left) Food Wrapping Material, (Right) Food Container
Table 1 Analytical Conditions
: Shim-pack XR-ODS Ⅱ (75 mmL. × 2.0 mmI.D., 2.2 μm)
: 0.1 % formic acid
: Methanol
: 25 %B (0 min) - 100 %B (2.5-7.5 min) - 25 %B (7.51-10 min)
: 0.5 mL/min
: 2 μL
: 40 °C
: SHIMADZU LCMS-8030
: +4.5 kV (ESI-Positive mode),
–3.5 kV (ESI-Negative mode)
Nebulizing Gas Flow : 1.5 L/min
Drying Gas Pressure : 10 L/min
: 250 °C
DL Temperature
: 400 °C
BH Temperature
For Research Use Only. Not for Use in Diagnostic Procedures.
SHIMADZU CORPORATION. International Marketing Division
6.0
0.8
Irganox 1010
Column
Mobile Phase A
Mobile Phase B
Gradient Program
Flow Rate
Injection Volume
Column Temperature
MS
Probe Voltage
5.5
1.0
0.0
5.0
5.0
1.2
1.0
1.5
0.0
3.5
(×100,000)
2.5
1.0
3.0
4.863
3.0
3.258
2.5
chromatograms of the substances detected. The
concentrations of each of the constituents calculated
using the calibration curves of Fig. 2 were determined
to be 49.4 ng/g of Irganox 1010 detected in the food
wrapping material, and 14.3 μg/g of the Irganox 245
and 48.7 ng/g of Irganox 1010 detected in the food
container.
3. Kanda-Nishikicho 1-chome, Chiyoda-ku, Tokyo 101-8448, Japan Phone: 81(3)3219-5641 Fax. 81(3)3219-5710
4.7
4.8
4.9
Irganox 1010
5.0

印刷見本‐2：「Part A 化合物ガイド」および「Part B 赤外吸収スペクトル