Analysis of Lipstick for Toxic Elements using ICP-MS

Transcription

Chemistry & Cosmetics
Analysis of Lipstick for Toxic Elements using ICP-MS
Patricia Atkins
Product Applications Specialist
© SPEX CertiPrep, Inc. 2011
Housekeeping
 Everyone in attendance today will receive a copy of the
presentation slides
 The webinar is being recorded and will be posted to our
YouTube account about one week after the event
 Questions will be answered at the end of the presentation
– Type any questions you may have into the question box
and we will answer them during the Q & A portion
History
 Cosmetics have historically contained
toxic compounds
 Egyptian cosmetics: Pb & Hg
– Kohl: burnt almonds, oxidized
copper, different-colored copper
ores, lead, ash, arsenic
compounds & ochre
– Mesdemet: copper and lead ore
 Greek & Romans
– White complexion = Pb
– Red colors = Cinnabar = Hg
– Brows = Stibium = Sb
History
 Medieval & Renaissance
– White Pale Complexion
= Mask of Youth
• Used by men &
women
• Hydroxide, carbonate
& Pb oxide
– Elizabeth I
• Covered acne and pox
scars with heavy white
makeup
History
 20th century
– Radium cosmetics & personal
products = ‘healthy glow’
• 1918
– Avg Salary = $1500
– Hourly wage= $0.30-$0.70
– Year rent $178
– $2 Compact = >$50 today
• 1930’s
– Radioactive materials
• 1950’s to today
– Spas with Radon
http://www.cosmeticsandskin.com
History
 Modern products perceptionno toxic compounds
– Recalls on FDA
– Various problems from
physical to bacterial
contamination
 Cosmetics used around the
globe
 Generates hundreds of
billions of dollars of revenue
Studies & Regulations
 FDA regulates cosmetic industry
– No premarket approval for
finished cosmetics
– Regulates limits on additives &
colorants
 Hepp et. Al = up to 3 ppm Pb
 This study examines the lipstick
for a wide range of compounds
and re-examines the Pb level
 Correlations examined between
colors, finish type and elemental
levels
Chemistry of Lipstick
 Base
– Waxes
– Oils
• Castor Oil
 Preservatives
– Vitamins
– Antioxidants
 Flavors
 Finish components
– Esters – shine
– Micas - shine
 Pigments & Colorants
Chemistry of Lipstick
 Pigments & Colorants
– Organic Colorants
• Coal Tar colorants
– must undergo safety
testing
– only ingredients required
by FDA
• FD&C colors – safe for
internal & external use
• External D&C – external use
– Inorganic Colorants in Lipstick
• Iron Oxide Black
• Iron Oxide Red
• Iron Oxide Orange
• Iron Oxide Yellow
• Iron Oxide Brown
• Manganese Violet
Samples
 48 Products from SPEX
CertiPrep Employees
 Age: new to several years old
 Price Range: $5 to $35 per
container
 14 Brands
 Products:
• Lip stains
• Lip gloss
• Lip balm
• Lipstick
Samples (cont.)
White/Colorless (6)
Beige/Tan (3)
Light Pink (3)
Brown (7)
Dark Pink (7)
Berry/Wine (11)
Corals/Peaches (11)
48 Samples
Samples (cont.)
 Four types of finishes
Pearlescent
Metallic
Matte
Pearlescent
Clear
 Three physical state types
–Solid
–Semi-solid
Metallic
–Liquid
Materials
 SPEX CertiPrep Standards:
• CLMS-1: Multi Element Solution Standard 1
• Base Oil 20 Standard
 Reagents:
• High Purity Nitric Acid
• High Purity Hydrofluoric Acid
• 4% Boric Acid Solution
Sample Preparation
 Hepp, N. M., Mindak, W. R., and Cheng,
J., Journal of Cosmetic Science, Vol. 60,
No. 4, July/August, 2009.
 Samples digested in CEM Mars 5
Microwave Unit
– XP-1500 Vessels
– two-step microwave digestion
procedure
Sample Preparation (cont.)
 Step 1:
– 0.3 g of sample
– 7 mL high purity Nitric Acid
– 2 mL high purity HF
– Microwave Program:
• Ramp to 130°C over 15
minutes; hold 3 minutes
• Ramp to 200°C over 15
minutes; hold 30 minutes
• Allow to cool
Sample Preparation (cont.)
 Step 2:
– 30 mL of 4% high purity
Boric Acid solution
– Microwave Program:
• Ramp to 170°C over
15 minutes; hold 10
minutes
 Diluted to 50 mL DI H2O
 Digestion blanks run prior
to sample digestion
 Diluted 1000x prior to ICPMS analysis
Instrument Conditions
 Instrumentation
– Macroelement analysis:
• PerkinElmer ICP-OES
Optima 7300
– Trace element analysis
• Agilent ICP-MS 7700
– Meinhard nebulizer
Condition
Setting
Power
1550 W
Plasma Gas
15 L/min
Aux Gas
0.3 L/min
Nebulizer
0.80 L/min
Sampling Rate
0.3 mL/min
– Cyclonic spray chamber
– Analysis performed
• normal mode: air
• collision mode: Helium
Elements Measured
Element
Ag
Al
As
Au
Ba
Be
Ca
Cd
Ce
Co
Cr
Cs
Cu
Cu
Fe
Ga
Gd
Ge
Hf
Hg
Ho
In
Ir
K
La
Li
Lu
Mg
Mn
Mo
Na
Nd
Gas Mode
Air
Air & He
Air & He
Air
Air
Air
He
He
Air
Air & He
Air & He
Air
He
He
He
Air
Air
He
Air
Air
Air
Air
Air
He
Air
Air
Air
Air
He
Air
Air
Air
Line
107, 109
27
75
197
135-137-138
9
44
111-113
140
59
52&53
133
63
63
56
71
156
74
178-180
201
165
115
193
39
139
7
175
24
55
95,97,98
23
146
Element
Ni
Os
P
Pb
Pd
Pr
Pt
Rb
Re
Rh
Ru
Sb
Sc
Se
Si
Sm
Sn
Sr
Ta
Tb
Te
Th
Ti
Tl
Tm
U
V
W
Y
Yb
Zn
Zr
Gas Mode
He & Air
Air
Air
Air
Air
Air
Air
Air
Air
Air
Air
Air
He
He
He
Air
He & Air
He & Air
Air
Air
Air
Air
Air
He
Air
Air
He
Air
Air
Air
He
Air
© SPEX
CertiPrep,
Line
60
189
31
206-208
105
141
195
85
187
103
101
121, 123
45
77
30
147
117-120
86 & 88
181
159
125
232
47
203, 205
169
238
51
182
89
172
66
Inc. 90
2011
Results: Trace Elements
 Precious metals and rare elements found in small
Element
Avg (ppm)
Max (ppm)
Ag
Au
0.04
0.02
0.21
0.22
Cu
1.47
7.20
Ga
Gd
Ge
2.01
0.03
0.25
4.28
0.15
1.37
Hf
0.15
1.13
In
0.07
0.95
Ir
0.47
3.62
La
0.40
1.29
Nd
0.07
0.68
– Au = Browns and Berries; multiple brands, one
predominant
Pd
Pr
Pt
0.02
0.01
0.03
0.10
0.10
0.74
– Pt = Whites and Browns but not in Berries;
predominate in one brand
Re
0.00
0.04
Rh
Se
Sm
0.03
0.13
0.03
0.21
0.52
0.13
– Pd = Berries & Dark Pinks
Ta
0.86
1.90
Th
W
Y
0.06
3.04
0.07
0.27
8.63
0.26
Yb
0.01
0.04
amounts
– Ag = 0.21 ppm
– Au = 0.22 ppm
– Pt = 0.74 ppm
 Correlations between colors
– Ag = Peach color; exclusively one brand
 Correlation between finishes
– Au = Metallic not Pearls
– Ag = Pearls not Metallic
– Ir = Pearls not Metallic
Results: Macroelements
Element
Al
Ba
Ca
Fe
K
Li
Lu
Mg
Mn
Na
P
Rb
Sc
Si
Sn
Sr
Ti
Zn
Avg (ppm)
38283.69
2734.56
28248.93
8262.90
11917.92
19.51
107.65
610.38
20.52
380.01
13.36
22.94
3.90
13387.93
21.77
30.28
14664.03
40.13
Max (ppm)
360,790.97
26,494.60
345,753.07
63,177.23
128,129.69
144.52
335.41
5,566.33
90.38
2,962.92
97.81
82.00
101.37
47,661.39
359.28
255.13
38,477.15
1,084.94
Zr
8.10
39.37
 Very high Al, Ca, K levels
– Concern over Al?
 Expect large amounts of Fe, K,
Mg, Si, Ti
Results: Macroelements (cont.)
160,000
140,000
Concentration (ppm)
120,000
White
100,000
Lt Pink
Dk Pink
80,000
Coral
60,000
Berry
Tan
40,000
Brown
20,000
0
Al
Ca
Fe
K
Si
Ti
Macroelement
1,800
1,600
1,400
Concentration (ppm)
1,200
White
Lt Pink
1,000
Dk Pink
800
Coral
Berry
600
Tan
Brown
400
200
0
Mg
Mn
Zn
Zr
Macroelement
Correlation with Color
– Darker colors, higher concentrations
•
•
•
•
•
•
Low Zr
Low Si
Cu
K
Mn
Se
•
•
•
•
•
•
•
•
• W
Al
Ca
Si
Zn
Cu
K
Mn
Se
•
•
•
•
•
•
Al
Ca
Si
Zn
P
Low Ca
• Zr
Correlation with Finish Type
Pearlescent
Matte
Metallic
Results: Toxic Elements
 Pb cited up to 3 ppm (Hepp et al)
– Our max = 2.4 ppm
Element
Avg
Min
Max
As
0.30
0
0.69
Be
0.49
ND
1.23
Ce
0.24
ND
3.37
Co
0.44
ND
4.30
– Cr = 31 ppm
Cr
2.44
0
31.45
– Ni = 23 ppm
Cs
1.68
ND
4.76
Mo
0.27
0
4.12
– V = 51 ppm
Ni
2.88
0
23.36
– Sb = 10 ppm
Pb
0.96
ND
2.39
Sb
0.33
ND
9.58
Tl
0.08
ND
0.23
V
4.68
ND
50.72
– Avg = 1 ppm
 Highest potentially toxic or
hazardous elements
 Low ppb levels found of Cd, Hg &
U
Results: Toxic Elements (< 1ppm)
0.90
0.80
Concentration (ppm)
0.70
White
0.60
Lt Pink
0.50
Dk Pink
0.40
Coral
0.30
Berry
Tan
0.20
Brown
0.10
0.00
As
Be
Ce
Mo
Tl
Trace Element
Results: Toxic Elements (<10 ppm)
8.00
7.00
Concentration (ppm)
6.00
White
5.00
Lt Pink
Dk Pink
4.00
Coral
3.00
Berry
Tan
2.00
Brown
1.00
0.00
Co
Cr
Cs
Ni
Pb
Sb
W
Trace Element
Results: Toxic Elements (<100 ppm)
100.00
90.00
80.00
Concentration (ppm)
70.00
White
60.00
Lt Pink
50.00
Dk Pink
Coral
40.00
Berry
30.00
Tan
20.00
Brown
10.00
0.00
Sn
Sr
V
Trace Element
Results: Toxic Elements (cont.)
Correlations with Color
Higher concentration = Darker colors
• V
• As
• V
• Sr
• As
• Pb
• Tl
• Pb
• Sr
• Pb
• Sr
Results: Toxic Elements (cont.)
Correlation with Finish Type
Pearlescent
Matte
Metallic
What does this mean?
Exposure & Human Limits
The EPA RfD – is the oral reference dosage
defined as: ‘…an estimate … of a daily exposure
to the human population (including sensitive
subgroups) that is likely to be without an
appreciable risk of deleterious effects during a
lifetime…expressed in units of milligrams per
kilogram of bodyweight per day (mg/kg/day).’
WHO - The TDI is an estimate of
the amount of a substance in food
or drinking-water, expressed on a
body weight basis (mg/kg or μg/kg
of body weight), that can be
ingested daily over a lifetime
without appreciable health risk.
Exposure
Element
Max
ug in 0.10 g
Concentration in
lipstick
Lipstick (ug/g)
Calculated Rfd for
EPA or WHO RfD
163-lb (74 kg)
Adult Female
(ug/kg/day)
(ug/kg)
Amount of lipstick
needed to exceed
RfD (g)
As
0.88
0.0088
4
296
334.54
Ba
26494.60
264.9460
200
14800
0.56
Be
1.17
0.0117
2
148
126.28
Cd
0.04
0.0004
1
74
1684.66
Cr
31.45
0.3145
3
222
7.06
Hg
0.08
0.0008
0.1
7.4
87.49
Ni
23.36
0.2336
20
1480
63.35
Pb
2.39
0.0239
3.6
266.4
111.39
Sb
9.58
0.0958
0.4
29.6
3.09
Sr
109.24
1.0924
600
44400
406.43
Tl
0.21
0.0021
0.1
7.4
34.66
U
0.05
0.0005
3
222
4639.80
V
36.43
0.3643
9
666
18.28
Exposure
Element
Amount of tubes of
lipstick consumed in
one day to exceed RfD
Ba
Sb
Tl
Hg
Pb
As
Cd
0.25
1
11
30
37
111
560
Conclusions
 Many elements found
present in lipstick
 Toxic elements
–Pb found up to 2 ppm
–Very Low Hg, Cd
found
 Very High amount of Al
Conclusions
 The highest concentrations of
elements in darker colors
 Light colors, glosses or balms
have lowest concentrations
 The exposure rate to the toxic
elements is very small
 Large amounts of lipstick would
have to be consumed to reach
RfD levels
Acknowledgements
 Thanks to all the employees of SPEX CertiPrep &
SamplePrep
 Huifang Lang, Chemist, SPEX CertiPrep
 Lazlo Ernyei, ICP Chemist, SPEX CertiPrep
 Bill Driscoll, ICP-MS Chemist, SPEX CertiPrep
 Vanaja Sivakumar, VP Inorganics, SPEX CertiPrep
 Method by Hepp, N. M., Mindak, W. R., and Cheng, J., Journal of
Cosmetic Science, Vol. 60, No. 4, July/August, 2009.
Questions?
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available on CD!
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standards kit for USP 232
(Part# USP-TXM1)
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Analysis of Lipstick for Toxic Elements using ICP-MS

Transcription

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