Chinese Journal of Chromatography ›› 2021, Vol. 39 ›› Issue (5): 552-557.DOI: 10.3724/SP.J.1123.2020.11003
• Technical Notes • Previous Articles
LÜ Wen*(), LI Hongying, LIU Jie, HAN Wei, HUANG Wei
Received:
2020-11-02
Online:
2021-05-08
Published:
2021-03-31
Contact:
LÜ Wen
CLC Number:
LÜ Wen, LI Hongying, LIU Jie, HAN Wei, HUANG Wei. Determination of 13 sunscreen agents in cosmetics by gas chromatography-mass spectrometry[J]. Chinese Journal of Chromatography, 2021, 39(5): 552-557.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2020.11003
No. | Compound | CAS No. | Retention time/min | Quantitative ion (m/z) | Qualitative ions (m/z) |
---|---|---|---|---|---|
1 | ES | 118-60-5 | 8.72 | 120 | 138, 121 |
2 | HMS | 118-56-9 | 10.09 | 138 | 69, 109 |
3 | 3-BC | 36861-47-9 | 10.94 | 128 | 240, 129 |
4 | BP-3 | 22071-24-5 | 12.52 | 227 | 151, 228 |
5 | IMC | 71617-10-2 | 12.58 | 178 | 161, 133 |
6 | 4-MBC | 36861-47-9 | 13.01 | 254 | 128, 115 |
7 | ED-PABA | 58817-05-03 | 16.44 | 165 | 148, 164 |
8 | EHMC | 5466-77-3 | 17.22 | 178 | 161, 133 |
9 | CBM | 52793-97-2 | 20.26 | 240 | 283, 134 |
10 | OC | 6197-30-4 | 22.64 | 204 | 232, 248 |
11 | BMDBM | 70356-09-1 | 24.25 | 310 | 135, 295 |
12 | DT | 155633-54-8 | 25.79 | 221 | 73, 369 |
13 | DHHB | 302776-68-7 | 28.77 | 382 | 397, 383 |
Table 1 Retention times, quantitative ions and qualitative ions of the 13 sunscreen agents
No. | Compound | CAS No. | Retention time/min | Quantitative ion (m/z) | Qualitative ions (m/z) |
---|---|---|---|---|---|
1 | ES | 118-60-5 | 8.72 | 120 | 138, 121 |
2 | HMS | 118-56-9 | 10.09 | 138 | 69, 109 |
3 | 3-BC | 36861-47-9 | 10.94 | 128 | 240, 129 |
4 | BP-3 | 22071-24-5 | 12.52 | 227 | 151, 228 |
5 | IMC | 71617-10-2 | 12.58 | 178 | 161, 133 |
6 | 4-MBC | 36861-47-9 | 13.01 | 254 | 128, 115 |
7 | ED-PABA | 58817-05-03 | 16.44 | 165 | 148, 164 |
8 | EHMC | 5466-77-3 | 17.22 | 178 | 161, 133 |
9 | CBM | 52793-97-2 | 20.26 | 240 | 283, 134 |
10 | OC | 6197-30-4 | 22.64 | 204 | 232, 248 |
11 | BMDBM | 70356-09-1 | 24.25 | 310 | 135, 295 |
12 | DT | 155633-54-8 | 25.79 | 221 | 73, 369 |
13 | DHHB | 302776-68-7 | 28.77 | 382 | 397, 383 |
Solvent | MEs/% | AR/% | ||||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 | 12 | 13 | ||
DCM | 94.1 | 96.1 | 93.7 | 90.1 | 96.0 | 99.5 | 93.4 | 92.3 | 93.7 | 93.2 | 98.5 | 99.7 | 100.5 | 96.3 |
MT | 82.4 | 88.8 | 87.3 | 87.4 | 87.8 | 93.9 | 76.2 | 85.5 | 97.5 | 83.2 | 93.3 | 89.1 | 94.0 | 89.2 |
ACN | 86.0 | 90.7 | 88.4 | 89.6 | 88.9 | 92.8 | 77.2 | 100.4 | 92.7 | 90.2 | 93.5 | 96.7 | 95.7 | 90.1 |
AT | 92.5 | 92.8 | 93.5 | 94.4 | 94.5 | 93.4 | 89.9 | 91.3 | 98.5 | 96.1 | 98.1 | 92.2 | 92.8 | 92.8 |
HA | 68.5 | 67.3 | 68.8 | 63.3 | 70.6 | 75.3 | 77.0 | 67.2 | 62.4 | 67.8 | 74.9 | 66.9 | 71.4 | 71.4 |
THF | 90.1 | 101.2 | 94.9 | 92.7 | 96.6 | 100.3 | 85.2 | 85.0 | 83.4 | 89.7 | 99.6 | 93.6 | 100.2 | 95.5 |
Table 2 Matrix effects (MEs) and average recoveries (ARs) of the 13 sunscreen agents with different extraction solvents
Solvent | MEs/% | AR/% | ||||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 | 12 | 13 | ||
DCM | 94.1 | 96.1 | 93.7 | 90.1 | 96.0 | 99.5 | 93.4 | 92.3 | 93.7 | 93.2 | 98.5 | 99.7 | 100.5 | 96.3 |
MT | 82.4 | 88.8 | 87.3 | 87.4 | 87.8 | 93.9 | 76.2 | 85.5 | 97.5 | 83.2 | 93.3 | 89.1 | 94.0 | 89.2 |
ACN | 86.0 | 90.7 | 88.4 | 89.6 | 88.9 | 92.8 | 77.2 | 100.4 | 92.7 | 90.2 | 93.5 | 96.7 | 95.7 | 90.1 |
AT | 92.5 | 92.8 | 93.5 | 94.4 | 94.5 | 93.4 | 89.9 | 91.3 | 98.5 | 96.1 | 98.1 | 92.2 | 92.8 | 92.8 |
HA | 68.5 | 67.3 | 68.8 | 63.3 | 70.6 | 75.3 | 77.0 | 67.2 | 62.4 | 67.8 | 74.9 | 66.9 | 71.4 | 71.4 |
THF | 90.1 | 101.2 | 94.9 | 92.7 | 96.6 | 100.3 | 85.2 | 85.0 | 83.4 | 89.7 | 99.6 | 93.6 | 100.2 | 95.5 |
Compound | Linear equation | r2 | Linear range/(mg/L) | LOD/(mg/g) | LOQ/(mg/g) | |
---|---|---|---|---|---|---|
ES | y=14236.13x-275.39 | 0.9982 | 0.25- | 7.5 | 0.05 | 0.17 |
HMS | y=8027.37x-483.33 | 0.9983 | 0.25- | 7.5 | 0.07 | 0.23 |
3-BC | y=7581.82x-1287.27 | 0.9996 | 0.25- | 7.5 | 0.06 | 0.20 |
BP-3 | y=10902.47x-339.78 | 0.9985 | 0.25- | 7.5 | 0.06 | 0.20 |
IMC | y=18269.94x+148.58 | 0.9993 | 0.25- | 7.5 | 0.05 | 0.17 |
4-MBC | y=5470.83x+384.16 | 0.9993 | 0.25- | 7.5 | 0.06 | 0.18 |
ED-PABA | y=17738.58x-952.17 | 0.9981 | 0.25- | 7.5 | 0.04 | 0.12 |
EHMC | y=18832.71x+271.52 | 0.9987 | 0.25- | 7.5 | 0.07 | 0.22 |
CBM | y=2603.48x-380.52 | 0.9989 | 1.25- | 37.5 | 0.26 | 0.87 |
OC | y=12870.92x-327.76 | 0.9984 | 1.25- | 37.5 | 0.18 | 0.60 |
BMDBM | y=5092.99x-482.54 | 0.9998 | 2.5- | 75 | 0.63 | 2.10 |
DT | y=4859.05x-609.55 | 0.9994 | 1.25- | 37.5 | 0.16 | 0.53 |
DHHB | y=5417.59x-786.16 | 0.9989 | 2.5- | 75 | 0.40 | 1.33 |
Table 3 Linear equations, linear ranges and LODs of the 13 sunscreen agents
Compound | Linear equation | r2 | Linear range/(mg/L) | LOD/(mg/g) | LOQ/(mg/g) | |
---|---|---|---|---|---|---|
ES | y=14236.13x-275.39 | 0.9982 | 0.25- | 7.5 | 0.05 | 0.17 |
HMS | y=8027.37x-483.33 | 0.9983 | 0.25- | 7.5 | 0.07 | 0.23 |
3-BC | y=7581.82x-1287.27 | 0.9996 | 0.25- | 7.5 | 0.06 | 0.20 |
BP-3 | y=10902.47x-339.78 | 0.9985 | 0.25- | 7.5 | 0.06 | 0.20 |
IMC | y=18269.94x+148.58 | 0.9993 | 0.25- | 7.5 | 0.05 | 0.17 |
4-MBC | y=5470.83x+384.16 | 0.9993 | 0.25- | 7.5 | 0.06 | 0.18 |
ED-PABA | y=17738.58x-952.17 | 0.9981 | 0.25- | 7.5 | 0.04 | 0.12 |
EHMC | y=18832.71x+271.52 | 0.9987 | 0.25- | 7.5 | 0.07 | 0.22 |
CBM | y=2603.48x-380.52 | 0.9989 | 1.25- | 37.5 | 0.26 | 0.87 |
OC | y=12870.92x-327.76 | 0.9984 | 1.25- | 37.5 | 0.18 | 0.60 |
BMDBM | y=5092.99x-482.54 | 0.9998 | 2.5- | 75 | 0.63 | 2.10 |
DT | y=4859.05x-609.55 | 0.9994 | 1.25- | 37.5 | 0.16 | 0.53 |
DHHB | y=5417.59x-786.16 | 0.9989 | 2.5- | 75 | 0.40 | 1.33 |
Compound | Spiked/ (mg/g) | Cream | Lotion | |||
---|---|---|---|---|---|---|
Recovery/ % | RSD/ % | Recovery/ % | RSD/ % | |||
ES | 1.25 | 94.5 | 1.9 | 94.2 | 2.5 | |
5 | 96.7 | 3.7 | 97.4 | 2.4 | ||
10 | 101.6 | 2.1 | 100.3 | 1.6 | ||
HMS | 2.5 | 95.1 | 2.7 | 92.5 | 2.8 | |
10 | 91.4 | 2.7 | 95.6 | 3.6 | ||
25 | 103.6 | 2.2 | 102.3 | 1.7 | ||
3-BC | 2.5 | 95.9 | 3.3 | 93.7 | 3.0 | |
10 | 94.4 | 2.4 | 94.1 | 2.8 | ||
25 | 94.8 | 3.4 | 92.7 | 1.2 | ||
BP-3 | 2.5 | 89.8 | 3.1 | 90.8 | 2.7 | |
10 | 90.7 | 2.6 | 91.9 | 2.3 | ||
25 | 90.8 | 3.2 | 89.8 | 1.7 | ||
IMC | 2.5 | 92.5 | 2.9 | 88.4 | 3.6 | |
10 | 89.7 | 2.9 | 93.6 | 2.1 | ||
25 | 91.1 | 3.0 | 89.8 | 1.8 | ||
4-MBC | 2.5 | 88.7 | 3.8 | 91.4 | 2.6 | |
10 | 95.9 | 1.7 | 98.9 | 1.6 | ||
25 | 93.7 | 2.7 | 92.4 | 1.6 | ||
ED-PABA | 2.5 | 91.5 | 3.7 | 92.7 | 3.9 | |
10 | 91.8 | 3.8 | 90.1 | 3.7 | ||
25 | 95.0 | 2.8 | 92.4 | 2.2 | ||
EHMC | 2.5 | 90.3 | 2.6 | 89.4 | 2.7 | |
10 | 89.7 | 2.7 | 89.7 | 2.7 | ||
25 | 92.9 | 2.4 | 95.0 | 1.9 | ||
CBM | 10 | 92.8 | 4.9 | 94.1 | 2.4 | |
40 | 89.7 | 2.6 | 89.4 | 3.1 | ||
100 | 92.6 | 3.4 | 94.0 | 1.7 | ||
OC | 10 | 89.5 | 4.7 | 89.3 | 2.6 | |
40 | 95.8 | 2.3 | 94.3 | 3.8 | ||
100 | 93.2 | 3.0 | 92.6 | 1.2 | ||
BMDBM | 25 | 94.7 | 3.5 | 90.3 | 2.7 | |
100 | 93.5 | 2.2 | 96.5 | 2.7 | ||
250 | 95.3 | 2.6 | 94.7 | 1.8 | ||
DT | 10 | 93.7 | 3.6 | 94.6 | 3.1 | |
40 | 94.8 | 2.9 | 95.2 | 3.0 | ||
100 | 94.8 | 3.5 | 93.2 | 2.5 | ||
DHHB | 25 | 95.7 | 2.4 | 91.7 | 2.8 | |
100 | 93.9 | 3.0 | 96.3 | 2.2 | ||
250 | 95.6 | 1.8 | 95.3 | 1.7 |
Table 4 Spiked recoveries and relative standard deviations of the 13 sunscreen agents (RSDs) (n=6)
Compound | Spiked/ (mg/g) | Cream | Lotion | |||
---|---|---|---|---|---|---|
Recovery/ % | RSD/ % | Recovery/ % | RSD/ % | |||
ES | 1.25 | 94.5 | 1.9 | 94.2 | 2.5 | |
5 | 96.7 | 3.7 | 97.4 | 2.4 | ||
10 | 101.6 | 2.1 | 100.3 | 1.6 | ||
HMS | 2.5 | 95.1 | 2.7 | 92.5 | 2.8 | |
10 | 91.4 | 2.7 | 95.6 | 3.6 | ||
25 | 103.6 | 2.2 | 102.3 | 1.7 | ||
3-BC | 2.5 | 95.9 | 3.3 | 93.7 | 3.0 | |
10 | 94.4 | 2.4 | 94.1 | 2.8 | ||
25 | 94.8 | 3.4 | 92.7 | 1.2 | ||
BP-3 | 2.5 | 89.8 | 3.1 | 90.8 | 2.7 | |
10 | 90.7 | 2.6 | 91.9 | 2.3 | ||
25 | 90.8 | 3.2 | 89.8 | 1.7 | ||
IMC | 2.5 | 92.5 | 2.9 | 88.4 | 3.6 | |
10 | 89.7 | 2.9 | 93.6 | 2.1 | ||
25 | 91.1 | 3.0 | 89.8 | 1.8 | ||
4-MBC | 2.5 | 88.7 | 3.8 | 91.4 | 2.6 | |
10 | 95.9 | 1.7 | 98.9 | 1.6 | ||
25 | 93.7 | 2.7 | 92.4 | 1.6 | ||
ED-PABA | 2.5 | 91.5 | 3.7 | 92.7 | 3.9 | |
10 | 91.8 | 3.8 | 90.1 | 3.7 | ||
25 | 95.0 | 2.8 | 92.4 | 2.2 | ||
EHMC | 2.5 | 90.3 | 2.6 | 89.4 | 2.7 | |
10 | 89.7 | 2.7 | 89.7 | 2.7 | ||
25 | 92.9 | 2.4 | 95.0 | 1.9 | ||
CBM | 10 | 92.8 | 4.9 | 94.1 | 2.4 | |
40 | 89.7 | 2.6 | 89.4 | 3.1 | ||
100 | 92.6 | 3.4 | 94.0 | 1.7 | ||
OC | 10 | 89.5 | 4.7 | 89.3 | 2.6 | |
40 | 95.8 | 2.3 | 94.3 | 3.8 | ||
100 | 93.2 | 3.0 | 92.6 | 1.2 | ||
BMDBM | 25 | 94.7 | 3.5 | 90.3 | 2.7 | |
100 | 93.5 | 2.2 | 96.5 | 2.7 | ||
250 | 95.3 | 2.6 | 94.7 | 1.8 | ||
DT | 10 | 93.7 | 3.6 | 94.6 | 3.1 | |
40 | 94.8 | 2.9 | 95.2 | 3.0 | ||
100 | 94.8 | 3.5 | 93.2 | 2.5 | ||
DHHB | 25 | 95.7 | 2.4 | 91.7 | 2.8 | |
100 | 93.9 | 3.0 | 96.3 | 2.2 | ||
250 | 95.6 | 1.8 | 95.3 | 1.7 |
Compound | Contents/% | ||||
---|---|---|---|---|---|
Cream 1 | Cream 2 | Lotion 1 | Lotion 2 | Lotion 3 | |
4-MBC | - | 2.6 | 1.6 | - | - |
EHMC | 4.1 | 3.6 | 3.1 | 4.3 | 5.2 |
OC | - | 3.6 | - | - | - |
BMDBM | - | 1.5 | - | - | - |
DHHB | - | - | 0.8 | - | - |
Table 5 Determination results of the samples
Compound | Contents/% | ||||
---|---|---|---|---|---|
Cream 1 | Cream 2 | Lotion 1 | Lotion 2 | Lotion 3 | |
4-MBC | - | 2.6 | 1.6 | - | - |
EHMC | 4.1 | 3.6 | 3.1 | 4.3 | 5.2 |
OC | - | 3.6 | - | - | - |
BMDBM | - | 1.5 | - | - | - |
DHHB | - | - | 0.8 | - | - |
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