Chinese Journal of Chromatography ›› 2022, Vol. 40 ›› Issue (6): 576-583.DOI: 10.3724/SP.J.1123.2021.11024
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XIAO Gengpeng1,2, YUAN Lu1,2, LUO Chunli1,2, LUO Xiang1,2, HUANG Yousheng1,2,*()
Received:
2021-11-28
Online:
2022-06-08
Published:
2022-05-26
Contact:
HUANG Yousheng
Supported by:
CLC Number:
XIAO Gengpeng, YUAN Lu, LUO Chunli, LUO Xiang, HUANG Yousheng. Simultaneous determination of seven dimethylcyclosiloxanes in cosmetics of different formulation systems by gel permeation chromatography purification-gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2022, 40(6): 576-583.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2021.11024
Compound | CAS No. | tR/ min | Ion pairs (m/z) | CEs/eV | Linear range/ (mg/L) | Linear equation | r |
---|---|---|---|---|---|---|---|
Hexamethylcyclotrisiloxane (D3) | 541-05-9 | 3.68 | 191.0/119.0* | 20, 15 | 0.05-1.0 | y=0.141x-0.771 | 0.994 |
207.1/191.1 | |||||||
Octamethylcyclotetrasiloxane (D4) | 556-67-2 | 5.74 | 265.1/249.1* | 10, 10 | 0.05-1.0 | y=0.401x+0.432 | 0.995 |
281.1/265.1 | |||||||
Decamethylcyclopentasiloxane (D5) | 541-02-6 | 7.98 | 267.0/251.1* | 15, 10 | 0.05-1.0 | y=0.320x-0.522 | 0.996 |
355.1/267.1 | |||||||
Dodecamethylcyclohexasiloxane (D6) | 540-97-6 | 9.52 | 341.1/73.1* | 15, 10 | 0.05-1.0 | y=0.101x+0.418 | 0.996 |
429.1/341.1 | |||||||
Tetradecamethylcycloheptasiloxane (D7) | 107-50-6 | 11.23 | 281.1/73.1* | 10, 15 | 0.05-1.0 | y=0.104x-0.106 | 0.994 |
281.1/265.1 | |||||||
Hexadecamethylcyclooctasiloxane (D8) | 556-68-3 | 12.58 | 355.1/73.1* | 10, 5 | 0.05-1.0 | y=0.449x-0.785 | 0.997 |
401.0/327.1 | |||||||
Octadecamethylcyclononasiloxane (D9) | 556-71-8 | 14.99 | 355.1/267.1* | 10, 10 | 0.05-1.0 | y=0.122x-0.333 | 0.998 |
429.1/341.1 | |||||||
n-Hexadecane (n-C16H34, IS) | 554-76-3 | 13.41 | 57.1/29.1* | 10, 5 | - | - | - |
71.1/43.1 |
Table 1 Retention times, quantitative ions, qualitative ions, linear equations and correlation coefficients (r) of dimethylcyclosiloxanes (DMCs) and internal standard (IS) substances
Compound | CAS No. | tR/ min | Ion pairs (m/z) | CEs/eV | Linear range/ (mg/L) | Linear equation | r |
---|---|---|---|---|---|---|---|
Hexamethylcyclotrisiloxane (D3) | 541-05-9 | 3.68 | 191.0/119.0* | 20, 15 | 0.05-1.0 | y=0.141x-0.771 | 0.994 |
207.1/191.1 | |||||||
Octamethylcyclotetrasiloxane (D4) | 556-67-2 | 5.74 | 265.1/249.1* | 10, 10 | 0.05-1.0 | y=0.401x+0.432 | 0.995 |
281.1/265.1 | |||||||
Decamethylcyclopentasiloxane (D5) | 541-02-6 | 7.98 | 267.0/251.1* | 15, 10 | 0.05-1.0 | y=0.320x-0.522 | 0.996 |
355.1/267.1 | |||||||
Dodecamethylcyclohexasiloxane (D6) | 540-97-6 | 9.52 | 341.1/73.1* | 15, 10 | 0.05-1.0 | y=0.101x+0.418 | 0.996 |
429.1/341.1 | |||||||
Tetradecamethylcycloheptasiloxane (D7) | 107-50-6 | 11.23 | 281.1/73.1* | 10, 15 | 0.05-1.0 | y=0.104x-0.106 | 0.994 |
281.1/265.1 | |||||||
Hexadecamethylcyclooctasiloxane (D8) | 556-68-3 | 12.58 | 355.1/73.1* | 10, 5 | 0.05-1.0 | y=0.449x-0.785 | 0.997 |
401.0/327.1 | |||||||
Octadecamethylcyclononasiloxane (D9) | 556-71-8 | 14.99 | 355.1/267.1* | 10, 10 | 0.05-1.0 | y=0.122x-0.333 | 0.998 |
429.1/341.1 | |||||||
n-Hexadecane (n-C16H34, IS) | 554-76-3 | 13.41 | 57.1/29.1* | 10, 5 | - | - | - |
71.1/43.1 |
Type | Sample | CDetected/(mg/L) | CQuantitative/(mg/L) | LOD/(mg/kg) | LOQ/(mg/kg) | |
---|---|---|---|---|---|---|
O/W cosmetics | hand cream | 0.01 | 0.03 | 0.04 | 0.12 | |
W/O cosmetics | foundation primer | 0.02 | 0.06 | 0.08 | 0.24 | |
Full oil type cosmetics | lip stick | 0.01 | 0.03 | 0.04 | 0.12 | |
Powdered cosmetics | rouge | 0.01 | 0.03 | 0.04 | 0.12 |
Table 2 Limits of detection (LODs) and limits of quantification (LOQs) of DMCs in cosmetics of different formulation systems
Type | Sample | CDetected/(mg/L) | CQuantitative/(mg/L) | LOD/(mg/kg) | LOQ/(mg/kg) | |
---|---|---|---|---|---|---|
O/W cosmetics | hand cream | 0.01 | 0.03 | 0.04 | 0.12 | |
W/O cosmetics | foundation primer | 0.02 | 0.06 | 0.08 | 0.24 | |
Full oil type cosmetics | lip stick | 0.01 | 0.03 | 0.04 | 0.12 | |
Powdered cosmetics | rouge | 0.01 | 0.03 | 0.04 | 0.12 |
Compound | Hand cream | Foundation primer | Lip stick | Rouge | ||||||||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
0.5 mg/kg | 1.0 mg/kg | 3.0 mg/kg | 0.5 mg/kg | 1.0 mg/kg | 3.0 mg/kg | 0.5 mg/kg | 1.0 mg/kg | 3.0 mg/kg | 0.5 mg/kg | 1.0 mg/kg | 3.0 mg/kg | |||||||||
D3 | 86.7 | 92.3 | 87.3 | 89.7 | 93.8 | 86.6 | 88.7 | 91.4 | 86.4 | 88.1 | 91.1 | 89.1 | ||||||||
D4 | 87.4 | 88.5 | 89.0 | 85.8 | 92.7 | 87.1 | 87.6 | 87.3 | 89.2 | 86.4 | 87.9 | 89.8 | ||||||||
D5 | 90.3 | 85.3 | 93.5 | 86.9 | 94.6 | 91.5 | 91.2 | 85.7 | 90.5 | 91.1 | 87.1 | 93.7 | ||||||||
D6 | 85.6 | 93.5 | 100.9 | 86.3 | 92.1 | 108.8 | 86.4 | 91.5 | 89.9 | 86.2 | 94.2 | 103.7 | ||||||||
D7 | 88.2 | 101.8 | 107.3 | 87.2 | 88.8 | 105.3 | 86.2 | 106.8 | 101.2 | 87.3 | 103.7 | 101.6 | ||||||||
D8 | 85.8 | 96.5 | 91.7 | 85.9 | 86.7 | 92.7 | 88.7 | 91.5 | 88.6 | 85.6 | 94.2 | 90.3 | ||||||||
D9 | 91.1 | 103.8 | 106.2 | 86.1 | 90.8 | 103.8 | 90.7 | 104.8 | 101.4 | 90.1 | 89.8 | 103.1 |
Table 3 Spiked recoveries of the seven DMCs in cosmetics of different formulation systems (n=6) %
Compound | Hand cream | Foundation primer | Lip stick | Rouge | ||||||||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
0.5 mg/kg | 1.0 mg/kg | 3.0 mg/kg | 0.5 mg/kg | 1.0 mg/kg | 3.0 mg/kg | 0.5 mg/kg | 1.0 mg/kg | 3.0 mg/kg | 0.5 mg/kg | 1.0 mg/kg | 3.0 mg/kg | |||||||||
D3 | 86.7 | 92.3 | 87.3 | 89.7 | 93.8 | 86.6 | 88.7 | 91.4 | 86.4 | 88.1 | 91.1 | 89.1 | ||||||||
D4 | 87.4 | 88.5 | 89.0 | 85.8 | 92.7 | 87.1 | 87.6 | 87.3 | 89.2 | 86.4 | 87.9 | 89.8 | ||||||||
D5 | 90.3 | 85.3 | 93.5 | 86.9 | 94.6 | 91.5 | 91.2 | 85.7 | 90.5 | 91.1 | 87.1 | 93.7 | ||||||||
D6 | 85.6 | 93.5 | 100.9 | 86.3 | 92.1 | 108.8 | 86.4 | 91.5 | 89.9 | 86.2 | 94.2 | 103.7 | ||||||||
D7 | 88.2 | 101.8 | 107.3 | 87.2 | 88.8 | 105.3 | 86.2 | 106.8 | 101.2 | 87.3 | 103.7 | 101.6 | ||||||||
D8 | 85.8 | 96.5 | 91.7 | 85.9 | 86.7 | 92.7 | 88.7 | 91.5 | 88.6 | 85.6 | 94.2 | 90.3 | ||||||||
D9 | 91.1 | 103.8 | 106.2 | 86.1 | 90.8 | 103.8 | 90.7 | 104.8 | 101.4 | 90.1 | 89.8 | 103.1 |
Compound | Hand cream | Foundation primer | Lip stick | Rouge | ||||||||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
0.5 mg/kg | 1.0 mg/kg | 3.0 mg/kg | 0.5 mg/kg | 1.0 mg/kg | 3.0 mg/kg | 0.5 mg/kg | 1.0 mg/kg | 3.0 mg/kg | 0.5 mg/kg | 1.0 mg/kg | 3.0 mg/kg | |||||||||
D3 | 4.5(5.2)# | 4.1(4.7) | 3.5(4.2) | 6.5(5.8) | 4.6(4.2) | 5.5(7.2) | 5.8(5.1) | 4.0(5.3) | 3.5(5.3) | 4.1(5.6) | 5.5(7.2) | 3.5(4.6) | ||||||||
D4 | 8.2(6.9) | 3.8(5.3) | 4.1(4.4) | 6.1(5.8) | 6.5(5.3) | 6.5(5.7) | 4.5(5.0) | 3.5(5.1) | 4.5(5.6) | 6.5(7.2) | 4.1(7.0) | 4.7(5.1) | ||||||||
D5 | 5.5(6.7) | 6.5(5.1) | 5.5(3.9) | 5.5(4.7) | 5.1(6.5) | 4.8(5.2) | 4.3(6.2) | 3.1(4.7) | 4.8(5.1) | 7.0(6.2) | 3.5(4.8) | 4.2(5.5) | ||||||||
D6 | 6.2(7.3) | 4.5(4.2) | 4.4(5.6) | 7.5(9.2) | 6.5(7.4) | 6.3(7.2) | 5.7(5.1) | 4.5(5.9) | 3.5(4.2) | 3.8(5.0) | 4.9(5.5) | 6.5(5.0) | ||||||||
D7 | 4.6(6.3) | 5.5(6.5) | 5.1(7.5) | 6.5(9.4) | 6.1(8.2) | 7.5(6.6) | 6.5(5.3) | 3.7(5.1) | 3.9(5.8) | 5.5(5.1) | 3.7(5.2) | 3.5(5.4) | ||||||||
D8 | 5.6(9.2) | 4.1(5.6) | 3.5(4.1) | 5.7(6.6) | 5.5(7.4) | 6.5(5.4) | 5.5(5.1) | 4.1(6.2) | 4.0(6.3) | 6.5(7.8) | 4.1(5.2) | 3.5(6.1) | ||||||||
D9 | 4.8(6.4) | 4.8(7.2) | 3.1(4.3) | 6.5(5.4) | 6.7(8.4) | 5.7(6.8) | 4.5(5.7) | 5.5(7.0) | 5.5(7.2) | 5.5(5.9) | 3.5(5.3) | 4.8(6.2) |
Table 4 Intra-day and inter-day precisions of the seven DMCs in cosmetics of different formulation systems (n=6) %
Compound | Hand cream | Foundation primer | Lip stick | Rouge | ||||||||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
0.5 mg/kg | 1.0 mg/kg | 3.0 mg/kg | 0.5 mg/kg | 1.0 mg/kg | 3.0 mg/kg | 0.5 mg/kg | 1.0 mg/kg | 3.0 mg/kg | 0.5 mg/kg | 1.0 mg/kg | 3.0 mg/kg | |||||||||
D3 | 4.5(5.2)# | 4.1(4.7) | 3.5(4.2) | 6.5(5.8) | 4.6(4.2) | 5.5(7.2) | 5.8(5.1) | 4.0(5.3) | 3.5(5.3) | 4.1(5.6) | 5.5(7.2) | 3.5(4.6) | ||||||||
D4 | 8.2(6.9) | 3.8(5.3) | 4.1(4.4) | 6.1(5.8) | 6.5(5.3) | 6.5(5.7) | 4.5(5.0) | 3.5(5.1) | 4.5(5.6) | 6.5(7.2) | 4.1(7.0) | 4.7(5.1) | ||||||||
D5 | 5.5(6.7) | 6.5(5.1) | 5.5(3.9) | 5.5(4.7) | 5.1(6.5) | 4.8(5.2) | 4.3(6.2) | 3.1(4.7) | 4.8(5.1) | 7.0(6.2) | 3.5(4.8) | 4.2(5.5) | ||||||||
D6 | 6.2(7.3) | 4.5(4.2) | 4.4(5.6) | 7.5(9.2) | 6.5(7.4) | 6.3(7.2) | 5.7(5.1) | 4.5(5.9) | 3.5(4.2) | 3.8(5.0) | 4.9(5.5) | 6.5(5.0) | ||||||||
D7 | 4.6(6.3) | 5.5(6.5) | 5.1(7.5) | 6.5(9.4) | 6.1(8.2) | 7.5(6.6) | 6.5(5.3) | 3.7(5.1) | 3.9(5.8) | 5.5(5.1) | 3.7(5.2) | 3.5(5.4) | ||||||||
D8 | 5.6(9.2) | 4.1(5.6) | 3.5(4.1) | 5.7(6.6) | 5.5(7.4) | 6.5(5.4) | 5.5(5.1) | 4.1(6.2) | 4.0(6.3) | 6.5(7.8) | 4.1(5.2) | 3.5(6.1) | ||||||||
D9 | 4.8(6.4) | 4.8(7.2) | 3.1(4.3) | 6.5(5.4) | 6.7(8.4) | 5.7(6.8) | 4.5(5.7) | 5.5(7.0) | 5.5(7.2) | 5.5(5.9) | 3.5(5.3) | 4.8(6.2) |
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