LAAN-A-LC-E145

Application News
Hig h Pe r fo r m a n c e L iq u id Chro m a to g ra p h y N o . L375

High Speed, High Resolution Analysis (Part 20)

Analysis of Preservatives in Cosmetics
Preservatives such as parabens and phenoxyethanol
are used to maintain the safety and quality of
cosmetics. Analysis of these constituents is generally
conducted using HPLC.
This Application News introduces an example of
high-speed analysis of preservatives found in
cosmetics using the Prominence UFLC ultra-fast LC
system with the Shim-pack XR-ODS high-speed,
high-resolution column.

■ Analysis of Standard Solution

mAU
Here, 12 substances that are frequently used as 80
preservatives in cosmetics (methylparaben, ethylparaben, 230 nm
isopropylparaben, propylparaben, isobutylparaben, 70
butylparaben, phenoxyethanol, chlorphenesin, salicylic 60
acid, benzoic acid, sorbic acid, and dehydroacetic 2
acid) were selected as the analytes. 50
1
Fig. 1 shows the results of analysis of a standard 40
mixture of these constituents (10 mg/L each, prepared 6
30
using methanol), using a 4 μL injection.* A photodiode 7
array detector was used as the detector. The peaks 20
of phenoxyethanol, chlorphenesin, salicylic acid, 10 4
benzoic acid and dehydroacetic acid were identified
using 230 nm, and those of sorbic acid and the parabens 0
were identified using 255 nm. Since separation of -10
benzoic acid and salicylic acid is difficult with an 0.0 0.5 1.0 1.5 2.0 2.5 3.0 min
acidic phosphate buffer solution, separation was
conducted using a citrate buffer solution with a pKa mAU
near benzoic acid. 150
3
Excellent linearity was obtained for all the constituents, 255 nm
with an R2 value of 0.9999 or greater in the concentration 125
range of 1 - 100 mg/L.
100

75
✽Chromatogram is shown with the background subtracted. 9 10
5 1112
8
50

25
Table 1 Analytical Conditions
Column : Shim-pack XR-ODS (75 mm L. × 3.0 mm I.D., 2.2 μm) 0
Mobile Phase : A: 5 mmol/L (Sodium) citrate buffer (pH4.2)
B: Acetonitrile -25
B Conc. 30 % (0-1.2 min) → 40 % (1.5 min) → 55 % (3.5 min) 0.0 0.5 1.0 1.5 2.0 2.5 3.0 min
Flow Rate : 1.0 mL/min
■ Peaks
Injection Vol. : 4 μL
1.Salicylic Acid, 2.Benzoic Acid, 3.Sorbic Acid, 4.Phenoxyethanol,
Column Temp. : 40 ˚C 5.Methylparaben, 6. Chlorphenesin, 7.Dehydroacetic Acid,
Detection : SPD-M20A at 230, 255 nm 8.Ethylparaben, 9.Isopropylparaben, 10.Propylparaben,
Flow Cell : Semi-micro cell 11.Isobutylparaben, 12.Butylparaben

Fig. 1 Chromatogram of a Standard Mixture of 12 Preservatives

(10 mg/L each)
No.L375

■ UV Spectra

mAU mAU mAU

200.0 225.0 250.0 275.0 300.0 325.0 350.0 375.0 nm 200.0 225.0 250.0 275.0 300.0 325.0 350.0 375.0 nm 200.0 225.0 250.0 275.0 300.0 325.0 350.0 375.0 nm
SorbicAcid Methylparaben Isopropylparaben
Benzoic Acid Chlorphenesin Propylparaben
Phenoxyethanol DehydroaceticAcid Isobutylparaben
Salicylic Acid Ethylparaben Butylparaben

Fig. 2 UV Spectra of Preservatives

■ Analysis of Cosmetics
Fig. 3 and 4 show examples of analysis of 2 commercial ultrasonic extraction, the samples were brought to
cosmetics (creams). Each sample was weighed out 100 mL each and passed through a membrane filter
to 1.0 g, and after adding methanol and performing (pore size: 0.22 μm).

mAU mAU
50

230 nm 230 nm
40 30
4
4
30
20

20
10 2
10
6
0
0

-10 -10
0.0 0.5 1.0 1.5 2.0 2.5 3.0 min 0.0 0.5 1.0 1.5 2.0 2.5 3.0 min
mAU mAU
100 70
255 nm 255 nm
60
75 5 5
50
40
50
30 10
3
25 20
8 12 8
10 11 10
0 0
-10
-25
0.0 0.5 1.0 1.5 2.0 2.5 3.0 min 0.0 0.5 1.0 1.5 2.0 2.5 3.0 min
■ Peaks ■ Peaks
4.Phenoxyethanol, 5.Methylparaben, 6. Chlorphenesin, 8.Ethylparaben 2.Benzoic Acid, 3.Sorbic Acid, 4.Phenoxyethanol, 5.Methylparaben
10.Propylparaben, 11.Isobutylparaben 12.Butylparaben 8.Ethylparaben, 10.Propylparaben

Fig. 3 Chromatogram of Cosmetic A Fig. 4 Chromatogram of Cosmetic B

[References]
1) Mori, Nakamura, Onuki, Terashima, Miyamoto, Ogino, and Saito : Annual Report of Tokyo Metropolitan Institute of Public Health, No. 58 (2007)

NOTES:
✽This Application News has been produced and edited using information that was available when the
data was acquired for each article. This Application News is subject to revision without prior notice.

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URL http://www.shimadzu.com

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