Rapid Analysis of Complex
Heterogeneous Mixtures for Active
Components in Cosmetic Products
G OA L
Streamline your workflow when monitoring mixtures
To employ Waters ® Atmospheric Solids
Analysis Probe (ASAP) as a sample inlet
for mass spectrometry to directly analyze
heterogeneous samples and eliminate
sample preparation.
in targeted analyses with ASAP, which provides mass
Commercial Anti-Wrinkle Cream
Commercial Anti-Wrinkle Cream
472
100
%
%
100
150
0
0.00
0.20
0.40
0.60
0.80
1.00
0
100
473
291
185 206
292
200
430
300
400
474
500
600
700
800
900
1000
Commercial Anti-Aging Cream
Commercial Anti-Aging Cream
472
100
100
473
%
150
%
229
291
290
311
0
0.00
100
0.20
0.40
0.60
0.80
1.00
Commercial Sunblock Cream
0
100
200
400
139
0.20
0.40
0.60
0.80
0
513
500
579 607
600
700
800
900
1000
312
310
472
230
Time
1.00
474
Commercial Sunblock Cream
311
100
229
0
0.00
371 405
300
%
Active components, such as UV absorbers
are widely used in formulated personal care
products, including sun block and over-thecounter facial creams. These components
are constantly under examination for quality
control, thermal stability or shelf life, and
photochemical stability. The sample matrix
is a heterogeneous complex mixture that
includes components as diverse as pigments,
oils, emulsions, and functional or active organic
chemicals. Typical analyses of these types
of materials include the use of conventional
analytical tools, such as NMR, LC, or LC/MS.
These techniques require time-consuming
workup procedures that include precipitation,
extraction, filtration, separation, and
evaporation. ASAP can provide mass spectra
of mixtures within seconds without sample
workup, which streamlines the workflow when
monitoring mixtures in targeted analysis.
workup required.
%
BA C K G RO U N D
spectra of mixtures within seconds – no sample
100
195
200
284
473
313
360
300
400
500
600
700
800
Figure 1. The complex sample spectra were recorded for the bulk sample without dilution,
extraction, or any sample pre-treatment. Note that both negative and positive ionization
were collected – positive ionization data are displayed.
900
m/z
1000
T H E S O LU T I O N
100
Avobenzone
100
0.20
100
0.40
0.60
0.80
1.00
0.40
0.60
0.80
1.00
0
0.20
100
Homeostate
%
0.20
0
0.40
0.60
0.80
1.00
0.60
0.80
1.00
0.60
0.80
1.00
0.80
Time
1.00
Homeostate
%
Homeostate
%
0
Avobenzone
%
%
0
0.20
0.40
0.60
0.80
1.00
0
0.20
0.40
100
100
100
0
0.20
0.40
0.60
0.80
1.00
0
D5
%
D5
%
%
D5
0.20
0.40
0.60
0.80
1.00
0
0.20
0.40
100
100
%
Octinoxate
0
0.20
0.40
0.60
0.80
Time
1.00
Commercial Anti-Wrinkle Cream
0
Octisalate
%
100
Octinoxate
%
A tandem quadrupole mass spectrometer with an
ASAP probe was used to analyze critical components
in formulated products, without the need for
extensive sample preparation or isolation of the
analyte from a heterogeneous matrix. The sample
was loaded onto a glass tube on the probe by dipping
its tip directly into the product mixture. The probe
was inserted into the MS source at atmospheric
pressure. Desolvation gas heated to 350 °C was
used to volatilize the analytes. Mass spectra were
acquired in two minutes using both APCi positive
and negative mass scan modes. The targeted
100
0.20
0.40
0.60
0.80
Time
1.00
Commercial Anti-Aging Cream
0
0.20
0.40
0.60
Commercial Sunblock Cream
Figure 2. Thermal desorption chromatograms for the target analyte list using MS/MS data. Each
thermal chromatogram was processed using a simple smoothing function to provide consistent
data over the acquisition range.
analytes were isolated from matrix interference
based on confirmatory fragmentation.
A complex data set is displayed in the collected
spectra, shown in Figure 1, which provide a
summation of information from a wide array of
product components. Utilizing a targeted workflow
approach, an evaluation of the data set focused
on expected and other typical components in the
various products.
Employing a wide array of collision conditions
for the target analyte list, the sample components
were analyzed to determine appropriate
fragmentation conditions.
Based on the collision cell conditions for each
component in the target analyte list, a schedule
of MRM scans was established. The samples
were then reanalyzed using the ASAP sampling
method, and the resulting thermal desorption
chromatograms were collected, as shown in
Figure 2.
Analysis of active ingredients in personal care products was routinely conducted
using ASAP as a mass spectrometer inlet with a total analysis time of two
minutes. This technique allowed for direct sample introduction, without the
need for sample preparation. Complex sample matrix interferences were easily
addressed with a targeted analysis using established fragmentation patterns
produced in the collision cell, which resulted in unique analyte detection.
S U M M A RY
■■
Using ASAP as a sample inlet for analysis of heterogeneous sample matrices
allows for collection of characteristic mass spectra and analysis of relative
concentration of components in a product mixture.
■■
This analytical approach can be used to monitor key ingredients, as well as
to profile product integrity.
■■
ASAP can provide critical data and increased analysis capacity with minimal
specialized operator training required to support researchers, as well as
production operations.
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©2011 Waters Corporation. Produced in the U.S.A.
September 2011 720004026EN LL-PDF
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