Mass Detection Solutions for Cosmetics Industry

©2015 Waters Corporation 1
Mass Detection for the Cosmetics Industry
Jane Cooper
Senior Applications Scientist
Chemical Materials Business Operations
Wilmslow, UK

Introduction
 Background
– Analytical challenges
 Mass detection
– Ease of Use
– Advantages
 Application examples
 Questions

An Ecosystem Focused on Innovation
Contract
Research
Organizations
(CRO)
Contract
Manufacturing
Organizations
(CMO)
Active
Ingredient
Suppliers
(Botanicals/
Synthetic
Molecules)
Raw
Materials
Suppliers
Cosmetics &
Personal Care
Company

Analytical Solutions for Cosmetics &
Personal Care

Analytical Challenges
 Raw Materials Testing
– Establishing Action and Safety
o Verification liability on manufacturers
o Testing materials from certain geographical regions
o Heavy metals in raw materials
o What is the cost to you of non-conforming goods?
 Active Ingredients
o What is it?
o How much?
o What else is in the plant extraction?

 Formulation
– Ensuring Performance and Characterisation
o Chemical Diversity
o Impurities, Allergens, Pesticides
o How many components in a cosmetic formulation?
 Quality Control
– Delivering Optimum Production Volume
o Ensuring batch-to-batch conformity
o How much does losing a batch of cosmetic cost?
o Time delay in bringing product to market?

 Safety and Regulatory Compliance
– Making Compliance Routine
o Protecting customers is Number 1 goal
o Different requirements for FDA and Europe
o Understanding the impact of packaging on product safety
• Non Intentionally Added Substances
o Allergens
• Utilising LC not just GC
• 0.001% leave on and 0.01% rinse off
o Pesticides
o Heavy metals in raw materials
o How much is the fine for getting this wrong?

 Counterfeit Detection
– Protecting brand identity
o How much does it cost the cosmetic industry?
 Data Management
– Leveraging the Power of Information
o What cost failing an FDA audit?
 Phytochemistry
– Rise of botanical ingredients
o Profile and understand composition
o Do we understand metabolite activity?

• DISPOSABLE APERATURE • ONE PIECE PROBE • AUTOMATIC CALIBRATION •REDUCED MAINTENANCE AND PROVEN ROBUSTNESS
Purposely innovated to eliminate
downtime...
Adjustment free
single piece
electrospray probe
Protected
detector orifice

Simply switch off after use....
READY TO USE IN UNDER TEN MINUTES
Integrated calibration can
be automatically performed
upon start up

Complementary & compatible….
Providing information-rich mass spectral data
Detector concept
Built to consider …
- Samples
- Separations
- Scientists
• 30-1250 DA • PRE-OPTIMIZED ES± • 20 HZ FS • 100 HZ SIR • 4 ORDERS •
INTUITIVE •

Return on investment....
 Streamlined workflows and improved lab
efficiency via accessible mass detection
 Significant measurable return on investment
– Low running costs
o Power consumption
o Service plan costs
o Simply turn off after use
o Laboratory space savings
 Standardise on QDa and achieve substantial
savings over typical ownership duration
• LOW RUNNING COSTS • 110 – 240 V • PUSH BUTTON USAGE •

 Provides mass data to separation scientists
 Compact, intuitive and simple to use
 Improving workflows and efficiency in every laboratory – giving
a guaranteed return on investment!

Benefits of Mass Detection for the
Cosmetics Industry
 Method development
– Aim: One peak = one compound
o Detect coelutions and peaks missed by optical detection
o Track peaks more effectively
 Sample profiling
– Aim: Identify components and quantify
o Process complex matrices and low level target compounds
o Improved selectivity, more sensitivity
 Synthetic chemistry
– Aim: Confirm product identity
o Improve turnaround of results
o Improve information available on impurities
 Purification
– Aim: Isolate pure compound
o Collect fewer fractions with increased confidence

The power of mass
detection…. Identify co-elutions
Detect non-chromophoric
analytes

For all your separations….

Track peaks, see
coelutions, see more
peaks
One peak, one component
Coelutions and missed peaks
Method Development….
• RISK MANAGEMENT • WORKFLOW STREAMLINING • PRODUCTIVITY •

Identify and quantify
Complex matrices & low levels
More selectivity, more sensitivity
Sample Profiling….
• QUALITY • WORKFLOW INTEGRATION • PRODUCTIVITY •

Results now
Confirm product
Delay to analysis
Synthetic Chemistry….
• WORKFLOW INTEGRATION • RESOURCE MANAGEMENT • DEADLINES •

Single fraction
Isolate compound
Purification….
• WORKFLOW INTEGRATION • RESOURCE MANAGEMENT • PRODUCTIVITY •
Multiple fractions

Improving sensitivity and selectivity
for primary aromatic amines....
 Highly legislated Inks and Dyes industry
– PAA’s suspected carcinogens
 Added benefits:
– Improved Signal-to-noise over UV
– Increased Selectivity – distinguishes components masked in UV
METHOD DEVELOPMENT

Time
-0.00 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00
AU
-2.5e-3
0.0
2.5e-3
5.0e-3
7.5e-3
1.0e-2
1.25e-2
1.5e-2
1.75e-2
2.0e-2
2.25e-2
2.5e-2
2.75e-2
3.0e-2
3.25e-2
3.5e-2
3.75e-2
-0.00 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00
AU
-1.5e-2
-1.0e-2
-5.0e-3
0.0
5.0e-3
1.0e-2
1.5e-2
2.0e-2
2.5e-2
3.0e-2
3.5e-2
4.0e-2
4.5e-2
5.0e-2
5.5e-2
5.865.03
4.73
4.53
3.61
0.33
0.30
0.98
0.54
0.70
0.83
2.09
1.49
2.78 2.90
3.47
3.88
4.33
3.96
5.42
7.53
6.37
6.11 7.00
7.88
8.42
9.30
5.29
3.80
1.27
0.54
0.26
0.73
0.98
2.37
2.18
3.44
4.94
4.624.22
4.46
5.19
5.07
6.74
5.41
6.00
8.02
7.37
7.13
7.51
8.07
9.28
Peak tracking with Primary
Aromatic Amines....
PAA
letter
Primary Aromatic Amines
A Aniline
B o-Toluidine
C 1,3-Phenylenediamine
D 2,4-Dimethylaniline
E 2,6-Dimethylaniline
F 2,4-Toluenediamine
G 2,6-Toluenediamine
H o-Anisidine
I 2-Methoxy-5-methylaniline
J 4-Methoxy-m-phenylenediamine
K 2-Naphtylamine
L 3-Amino-4-methylbenzamide
M 1,5-Diaminonaphtalene
N 4-Aminobiphenyl
O 2-Aminobiphenyl
P Benzidine
Q 4-Chloro-2,5-dimethoxyaniline
R 4-Aminoazobenzol
S 4,4'-Methylenedianiline
T 3,3'-Dimethylbenzidine
U 4,4'-Thioaniline
V o-Aminoazotoluene
W 4,4'- Diamino-3,3'-dimethylbiphenylmethane
X o-Dianisidine
ACQUITY UPLC BEH Phenyl ,
1.7 µm, 2.1 x 50 mm
ACQUITY BEH C18,
1.7 µm, 2.1 x 50mm
A
U
J
I
H
G/L
F
D/E
C
B
M
R
V
P
N
W
K/T/X
S
O
Q
A
G/L
J
F
H
T
D/E
C
U
M W
V
P
N
X/Q
S/I
R
B
K
Reducing method
development times

Time
-0.00 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00
AU
-2.5e-3
0.0
2.5e-3
5.0e-3
7.5e-3
1.0e-2
1.25e-2
1.5e-2
1.75e-2
2.0e-2
2.25e-2
2.5e-2
2.75e-2
3.0e-2
3.25e-2
3.5e-2
3.75e-2
-0.00 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00
AU
-1.5e-2
-1.0e-2
-5.0e-3
0.0
5.0e-3
1.0e-2
1.5e-2
2.0e-2
2.5e-2
3.0e-2
3.5e-2
4.0e-2
4.5e-2
5.0e-2
5.5e-2
5.865.03
4.73
4.53
3.61
0.33
0.30
0.98
0.54
0.70
0.83
2.09
1.49
2.78 2.90
3.47
3.88
4.33
3.96
5.42
7.53
6.37
6.11 7.00
7.88
8.42
9.30
5.29
3.80
1.27
0.54
0.26
0.73
0.98
2.37
2.18
3.44
4.94
4.624.22
4.46
5.19
5.07
6.74
5.41
6.00
8.02
7.37
7.13
7.51
8.07
9.28
Peak tracking with Primary
Aromatic Amines....
ACQUITY UPLC BEH Phenyl ,
1.7 µm, 2.1 x 50 mm
ACQUITY BEH C18,
1.7 µm, 2.1 x 50mm
A
U
J
I
H
G/L
F
D/E
C
B
M
R
V
P
N
W
K/T/X
S
O
Q
A
G/L
J
F
H
T
D/E
C
U
M W
V
P
N
X/Q
S/I
R
B
K
Reducing method
development times
Time
4.10 4.15 4.20 4.25 4.30 4.35 4.40 4.45 4.50 4.55 4.60 4.65 4.70 4.75 4.80 4.85 4.90 4.95 5.00 5.05 5.10 5.15 5.20
AU
0.0
5.0e-3
1.0e-2
1.5e-2
2.0e-2
2.5e-2
4.10 4.15 4.20 4.25 4.30 4.35 4.40 4.45 4.50 4.55 4.60 4.65 4.70 4.75 4.80 4.85 4.90 4.95 5.00 5.05 5.10 5.15 5.20
%
16
4.10 4.15 4.20 4.25 4.30 4.35 4.40 4.45 4.50 4.55 4.60 4.65 4.70 4.75 4.80 4.85 4.90 4.95 5.00 5.05 5.10 5.15 5.20
%
0
4.62
4.64
4.09
4.23 4.37
5.154.81
4.94
4.624.22
4.46
4.81
5.19
5.07
I
S
4,4'-Methylenedianiline
UV chromatogram
(260 nm)
QDa chromatogram (m/z = 199)
QDa chromatogram (m/z = 138)
2-Methoxy-5-methylaniline
nm
200 220 240 260 280 300 320 340
AU
0.0
2.0e-2
4.0e-2
6.0e-2
8.0e-2
1.0e-1
1.2e-1
1.4e-1
1.6e-1
1.8e-1
nm
200 220 240 260 280 300 320 340
AU
0.0
2.0e-2
4.0e-2
6.0e-2
8.0e-2
1.0e-1
1.2e-1
1.4e-1
1.6e-1
206
290
202
244
2-Methoxy-5-methylaniline
4,4'-Methylenedianiline
I
S

UPC2 – Convergence Chromatography
 Simplify the analytical workflow
– Access robust normal phase separations
– Eliminate solvent exchange steps for organic extracts
 Deal with compound Similarity challenges
– Positional isomers (differ in location of functional groups)
– Chiral Separations (enantiomers & diastereomers)
 Deliver Orthogonal separations
– Different relative retention ensures full characterization
– Check method specificity by comparison to a second procedure
– Reveal “hidden” impurity or degradation peaks
– Increase confidence in characterization of complex samples

UPC2/QDa – Enhancing already
powerful and orthogonal separations

Chiral purity of propiconazole using
UPC2/QDa....
Rapid separation of diasteroisomers
AU
0.00
0.05
0.10
0.15
0.20
0.25
AU
0.00
0.02
0.04
0.06
0.08
Minutes
0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50 6.00 6.50 7.00
AU
-0.005
0.000
0.005
0.010
0.015
0.020
0.025
0.030
0.035
AU
-0.002
0.000
0.002
0.004
0.006
0.008
0.010
Minutes
4.00 4.50 5.00
AU
-0.005
0.000
0.005
0.010
0.015
0.020
0.025
0.030
0.035
AU
-0.002
0.000
0.002
0.004
0.006
0.008
0.010
Minutes
4.00 4.50 5.00
1
2
3 Formulation
sample
UV at 220 nm
Propiconazole
standard
4
5 86 7
1 2
3 4
5 8
6
7
SAMPLE PROFILING

Chiral purity using UPC2/QDa....
Linking mass detection to PDA data
Empower Mass Analysis window
1 2
3 4
5 6 7 8
UV
TIC
XIC
1 2 3
UV and MS spectra
4
UV spectra
Mass spectra

Chiral purity using UPC2/QDa....
Improved selectivity and sensitivity
PDA and mass chromatograms
AU
0.00
0.05
0.10
0.15
0.20
0.25
Intensity
0.0
2.0x10
8
4.0x10
8
6.0x10
8
8.0x10
8
1.0x10
9
1.2x10
9
1.4x10
9
1.6x10
9
Minutes
0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50 6.00 6.50
PDA 220 nm
XIC m/z 342
1
2
3 4
5
8
6 7
1
2
3 4
5 86 7
AU
-0.010
0.000
0.010
0.020
0.030
0.040
Intensity
-5.0x10
7
0.0
5.0x10
7
1.0x10
8
1.5x10
8
2.0x10
8
2.5x10
8
Minutes
4.00 5.00
AU
-0.010
0.000
0.010
0.020
0.030
0.040
Intensity
-5.0x10
7
0.0
5.0x10
7
1.0x10
8
1.5x10
8
2.0x10
8
2.5x10
8
Minutes
4.00 5.00
AU
-0.010
0.000
0.010
0.020
0.030
0.040
Intensity
-5.0x10
7
0.0
5.0x10
7
1.0x10
8
1.5x10
8
2.0x10
8
2.5x10
8
Minutes
4.00 5.00
PDA 220 nm
XIC m/z 342
5 86 7
AU
-0.010
0.000
0.010
0.020
0.030
0.040
Intensity
-5.0x10
7
0.0
5.0x10
7
1.0x10
8
1.5x10
8
2.0x10
8
2.5x10
8
Minutes
4.00 5.00

Is my peak pure….?
“My peak looked pure,
but the core MS lab
found otherwise”
Apex
Trailing
Check peak purity
using both mass
and PDA data
in Empower®
Leading

ACQUITY QDa Detector application
notes....

– Direct Analysis in Real Time
o DART is a desorption APCI ionisation
technique where a heated ionised gas is
directed at a target between the DART
interface and the QDa
o Ionises molecules from the surface of a
solid (e.g. tablet, food stuff, powder) or a
liquid (e.g. beverage)
o If the molecule can be ionized by ESI or
APCI it will work using DART
o Produces simple mass spectra as no
adducts are formed
DART/QDa
2005 Editors’ Gold
Award for Best Product
Compatible with
MassLynx software

Sample introduction options for
QDa/DART interface....
Direct manual analysis
Direct analysis of solid or
liquid samples
DART-OS
Sample applied to
OpenSpot card which is
aligned in the DART-OS
source for analysis

Automated sample introduction on
DART/QDa...
DART-SVP
Allows analysis of multiple
samples using single axis
automation
Sample holding options for DART-SVP
• Multiple tablet holder
• TLC plate holder
• Tweezer module
• Adapter for solid phase micro extraction
(SPME) tips
• Adapter for up to 12 DIP-it tips

 4 species of cinnamon
– Ceylon or true cinnamon
– Indonesian cinnamon
– Saigon cinnamon
– Chinese cinnamon
 Ceylon is the only species that does not
contact high concentration of coumarin
 Coumarin is linked to liver damage
 True cinnamon is more expensive and other
cinnamons are commonly used as
alternatives
 Labelling often does not disclose species of
cinnamon
Example DART/QDa Applications:
Analysis of Cinnamons for Adulteration

Direct analysis of Cinnamon Sticks…
“True Cinnamon”
Indonesian cinnamon

Direct analysis of Cinnamon Sticks…
“True Cinnamon”
Indonesian cinnamon
147
Coumarin
133
Cinnamaldehyde
133
Cinnamaldehyde
147
Coumarin

Analysis of ground cinnamons using
DART-SVP/QDa…
Cinnamaldehyde
133 m/z
Coumarin
147 m/z
Methyl Cinnamate
163 m/z

Analysis of ground cinnamons using
DART-SVP/QDa…
True
cinnamon
Indonesian
cinnamon
Saigon
cinnamon
Cinnamaldehyde
133 m/z
Coumarin
147 m/z
Methyl Cinnamate
163 m/z

 Cosmetics formulations are complex:
– Creams
– Lotions
– Powders
 Each formulation has a wide chemical
diversity:
– Functional polymers
– Detergents
– Fungicides
– Colourants
– Fragrance
– Conditioning agents
 Important to screen for presence of:
– Impurities
– Allergens
– Pesticides
Ensuring Product Performance and
Characterisation
Five commercial sources of Goldenseal
acquired for characterization

 Separation of five different
sources of Goldenseal
 2 main component peaks (A and
B) were identified as hydrastine
and berberine, respectively
– 5 other compounds also identified
Characterizing Goldenseal using
ACQUITY QDa Detection
Zoomed in UV chromatograms

 No two samples show exactly the
same compounds at the same
concentrations :
– Easily fingerprint each sample
– Compare formulations from
different manufacturers as well as
different sources of plant
 Rapid separation of complex
sample enabled by high efficiency
CORTECS columns
 Combining UV with mass data
gives a full characterization of
each sample with minimal effort
Characterizing Goldenseal using
ACQUITY QDa Detection
Identification of UV peaks in the liquid sample by
m/z value
A
B

Accessible MS-directed
purification....
PURIFICATION
Analytical screening
User defines criteria to
determine whether
purification is needed
AUTOMATED
PURIFICATION USING
AUTOPURIFY

purification....
PURIFICATION
Preparative Isolation
MS-directed purification collects target
analyte only

purification....
PURIFICATION
Analytical Purity Confirmation
Fraction tested to confirm higher purity

Simple, accurate purification....
2.00 4.00 6.00
m/z
250 500
%
0
100
145.2
m/z
250 500
%
0
100
242.3
m/z
250 500
%
0
100
m/z
250 500
%
0
100
279.4

Simple, accurate purification....
2.00 4.00 6.00

Benefits of Mass Detection for the
Cosmetics Industry
 Method development
– Aim: One peak = one compound
o Detect coelutions and peaks missed by optical detection
o Track peaks more effectively
 Sample profiling
– Aim: Identify components and quantify
o Process complex matrices and low level target compounds
o Improved selectivity, more sensitivity
 Synthetic chemistry
– Aim: Confirm product identity
o Improve turnaround of results
o Improve information available on impurities
 Purification
– Aim: Isolate pure compound
o Collect fewer fractions with increased confidence

Any Questions?

Mass Detection Solutions for Cosmetics Industry

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