China Surfactant Detergent & Cosmetics ›› 2023, Vol. 53 ›› Issue (4): 481-486.doi: 10.3969/j.issn.1001-1803.2023.04.016
• Analytical methods and testing • Previous Articles Next Articles
Wu Yuanyang*(),Zhang Liyuan,Wang Ren,He Tingting
Received:
2022-04-02
Revised:
2023-03-14
Online:
2023-04-22
Published:
2023-04-25
Contact:
* Tel.: +86-0571-87180330, E-mail: CLC Number:
Wu Yuanyang, Zhang Liyuan, Wang Ren, He Tingting. Determination of 10 prohibited stines in 3 different matrixes of cosmetics by HPLC-MS/MS[J].China Surfactant Detergent & Cosmetics, 2023, 53(4): 481-486.
Tab. 1
Retention times and MS/MS parameters of 10 stines drugs"
No. | Compound | Retention time/min | Precursorion(m/z) | Product ions (m/z) | Fragmentor/eV | CE/eV |
---|---|---|---|---|---|---|
1 | Ebastine | 8.393 | 470.4 | 167.0*,203.0 | 135 | 25,30 |
2 | Betahistine dihydrochloride | 2.042 | 137.2 | 94.0*,106.0 | 100 | 8,10 |
3 | Acrivastine | 6.638 | 349.2 | 278.0*,260.0 | 135 | 10,25 |
4 | Azelastine hydrochloride | 7.377 | 382.2 | 112.0*, 58.1 | 135 | 25,50 |
5 | Mizolastine | 7.871 | 433.3 | 108.9*,308.0 | 135 | 45,20 |
6 | Epinastine hydrochloride | 6.088 | 250.2 | 193.0*, 91.0 | 135 | 35,35 |
7 | Setastine hydrochloride | 8.003 | 358.2 | 215.0*,136.9 | 135 | 10,40 |
8 | Emedastine difumarate | 5.250 | 303.2 | 246.1*, 71.9 | 135 | 20,30 |
9 | Clemastine fumarate | 8.027 | 344.2 | 215.0*,130.0 | 100 | 15, 8 |
10 | Bepotastine besylate | 6.807 | 389.2 | 167.0*,201.9 | 135 | 50,20 |
Tab. 2
Linear regression equation, detection limit and quantification limit of 10 stines drugs"
No. | Compound | Linear equation | Linear range/(μg/L) | LOD/(μg/L) | LOQ/(μg/L) |
---|---|---|---|---|---|
1 | Ebastine | y=13 515.28x+1 615.27 | 0.1~1.6 | 0.003 | 0.011 |
2 | Betahistine dihydrochloride | y=964.30x-98.62 | 1~16 | 0.12 | 0.39 |
3 | Acrivastine | y=7 123.00x+433.91 | 0.1~1.6 | 0.008 | 0.026 |
4 | Azelastine hydrochloride | y=8 836.62x+74.87 | 0.1~1.6 | 0.013 | 0.043 |
5 | Mizolastine | y=4 668.40x-1 433.94 | 1~16 | 0.030 | 0.10 |
6 | Epinastine hydrochloride | y=961.00x-167.34 | 1~16 | 0.037 | 0.12 |
7 | Setastine hydrochloride | y=10 380.71x-155.78 | 0.1~1.6 | 0.021 | 0.070 |
8 | Emedastine difumarate | y=1 491.56x-764.85 | 1~16 | 0.076 | 0.25 |
9 | Clemastine fumarate | y=5 679.22x+240.55 | 0.1~1.6 | 0.008 | 0.025 |
10 | Bepotastine besylate | y=3 245.71x+12.93 | 0.1~1.6 | 0.009 | 0.029 |
Tab. 3
Recovery rate and precision of 10 stines drugs in different matrixes (n=6)"
No. | Compound | Spiked level/(mg/kg) | Average recoveries (RSDs)/% | ||
---|---|---|---|---|---|
Water aqua | Lotion | Cream | |||
1 | Ebastine | 0.2 | 89.8(2.77) | 88.1(2.83) | 88.9(3.78) |
0.4 | 103.2(1.39) | 93.9(4.72) | 92.2(3.38) | ||
1.0 | 106.0(2.24) | 92.0(0.44) | 87.8(1.52) | ||
2 | Betahistine dihydrochloride | 2 | 99.0(4.87) | 95.2(3.99) | 88.8(1.96) |
4 | 90.2(0.32) | 90.1(1.73) | 88.8(1.79) | ||
10 | 91.9(1.69) | 97.6(2.76) | 87.1(0.78) | ||
3 | Acrivastine | 0.2 | 101.9(1.61) | 97.4(4.29) | 94.5(4.48) |
0.4 | 100.2(4.55) | 99.4(2.85) | 101.5(4.62) | ||
1.0 | 107.8(1.61) | 104.3(2.14) | 103.3(3.96) | ||
4 | Azelastine hydrochloride | 0.2 | 92.2(4.92) | 87.1(0.76) | 101.9(4.52) |
0.4 | 91.5(2.78) | 90.6(1.49) | 95.5(4.46) | ||
1.0 | 89.4(3.96) | 89.1(1.22) | 98.9(3.72) | ||
5 | Mizolastine | 2 | 93.1(2.03) | 93.6(1.78) | 104.2(0.61) |
4 | 90.9(1.33) | 90.9(1.81) | 92.0(1.75) | ||
10 | 88.0(0.52) | 90.6(2.16) | 90.6(2.73) | ||
6 | Epinastine hydrochloride | 2 | 104.4(2.36) | 103.8(4.95) | 106.8(1.33) |
4 | 104.6(1.69) | 104.2(2.03) | 105.0(1.21) | ||
10 | 103.4(2.91) | 104.1(0.61) | 106.0(0.52) | ||
7 | Setastine hydrochloride | 0.2 | 104.0(2.51) | 91.3(1.31) | 100.0(2.73) |
0.4 | 92.9(3.88) | 90.7(1.61) | 89.9(3.52) | ||
1.0 | 91.4(1.43) | 91.0(1.98) | 90.1(4.75) | ||
8 | Emedastine difumarate | 2 | 102.0(4.60) | 106.5(0.83) | 107.7(0.87) |
4 | 90.0(1.85) | 95.9(3.26) | 96.4(4.41) | ||
10 | 88.4(2.58) | 99.8(1.07) | 97.6(2.23) | ||
9 | Clemastine fumarate | 0.2 | 99.1(4.02) | 88.3(2.55) | 88.3(1.15) |
0.4 | 94.0(2.74) | 91.1(4.65) | 92.2(2.64) | ||
1.0 | 98.4(1.49) | 90.1(3.68) | 91.7(4.79) | ||
10 | Bepotastine besylate | 0.2 | 95.9(4.58) | 90.7(0.21) | 97.2(1.89) |
0.4 | 94.9(2.94) | 91.9(3.85) | 102.7(3.01) | ||
1.0 | 88.5(2.52) | 88.7(2.79) | 88.9(2.07) |
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