China Surfactant Detergent & Cosmetics ›› 2023, Vol. 53 ›› Issue (6): 714-720.doi: 10.3969/j.issn.2097-2806.2023.06.014
• Analytical methods and testing • Previous Articles Next Articles
Sun Xiaojie*(),Wang Yumei,Liu Zhen,Liu Qinan
Received:
2022-05-12
Revised:
2023-05-31
Online:
2023-06-22
Published:
2023-06-25
Contact:
*Tel.: +86-18951783108, E-mail: CLC Number:
Sun Xiaojie, Wang Yumei, Liu Zhen, Liu Qinan. Determination of 17 cephalosporins residues in cosmetics by HPLC-MS-MS[J].China Surfactant Detergent & Cosmetics, 2023, 53(6): 714-720.
Tab. 1
MS parameters of 17 cephalosporins"
序号 | 化合物名称 | 保留时间/min | 母离子(m/z) | 子离子(m/z) | 碰撞电压/V | 裂解电压/V |
---|---|---|---|---|---|---|
1 | 去乙酰头孢匹林 | 2.36 | 382.2 | 11.8*,152.0 | 20,10 | 90 |
2 | 头孢吡肟 | 3.26 | 481.1 | 86.0*,166.9 | 15,25 | 80 |
3 | 头孢米诺 | 4.14 | 520.0 | 214.8*,161.0 | 15,20 | 100 |
4 | 头孢羟氨苄 | 4.32 | 364.0 | 113.9*,157.9 | 13,20 | 90 |
5 | 头孢匹林 | 4.65 | 424.4 | 152.0*,292.2 | 20,14 | 100 |
6 | 头孢他啶 | 4.73 | 547.1 | 166.9*,396.0 | 26,16 | 100 |
7 | 头孢洛宁 | 5.08 | 459.3 | 151.9*,337.1 | 18,10 | 80 |
8 | 头孢地尼 | 5.17 | 396.0 | 125.9*,227.0 | 30,12 | 80 |
9 | 头孢克洛 | 5.38 | 368.0 | 106.0*,173.9 | 22,15 | 110 |
10 | 头孢噻肟 | 5.57 | 456.4 | 296.2*,167.0 | 18,10 | 120 |
11 | 头孢克肟 | 5.69 | 454.0 | 126.0*,285.0 | 15,10 | 110 |
12 | 头孢唑林 | 5.72 | 455.3 | 156.0*,323.2 | 16,10 | 120 |
13 | 头孢匹胺 | 5.87 | 613.1 | 257.1*,285.1 | 25,21 | 100 |
14 | 头孢拉定 | 5.88 | 350.2 | 158.0*,176.1 | 12,18 | 120 |
15 | 头孢哌酮 | 5.93 | 646.5 | 143.1*,290.1 | 32,24 | 100 |
16 | 头孢孟多 | 6.41 | 463.1 | 158.0*,347.0 | 16,4 | 80 |
17 | 头孢他美酯 | 7.96 | 512.1 | 241.0*,398.1 | 24,30 | 120 |
Tab. 2
Linear ranges and correlation coefficients of 17 cephalosporins"
序号 | 水剂 | 油剂 | 膏霜类 | 线性范围/(ng/g) | |||||
---|---|---|---|---|---|---|---|---|---|
线性方程 | R2 | 线性方程 | R2 | 线性方程 | R2 | ||||
1 | y=581.3x-652.3 | 0.999 3 | y=10 936.4x-42 497.9 | 0.993 2 | y=4 509.9x-117.4 | 0.994 4 | 10~200 | ||
2 | y=2 110.7x+414.5 | 0.999 2 | y=12 156.2x-39 488.9 | 0.991 4 | y=2 110.9x+74.1 | 0.993 4 | 10~200 | ||
3 | y=5 014.1x+528.6 | 0.998 1 | y=37 113.12x-1 740.6 | 0.994 3 | y=3 475.6x-80.3 | 0.997 3 | 10~200 | ||
4 | y=4 671.4x-5 023.8 | 0.998 7 | y=3 190.2x-13 374.2 | 0.993 9 | y=1 094.0x-14.3 | 0.991 8 | 30~300 | ||
5 | y=1 383.6x-1 871.1 | 0.998 6 | y=7 055.9x-26 152.5 | 0.993 3 | y=2 320.6x+184.9 | 0.993 2 | 30~300 | ||
6 | y=229.4x-48.5 | 0.997 3 | y=1 814.3x-72.7 | 0.993 7 | y=1 164.3x-49.1 | 0.996 7 | 10~200 | ||
7 | y=5 801.7x-4 153.8 | 0.999 2 | y=2 427.09 x -72.5 | 0.999 2 | y=1 223.2x-33.7 | 0.993 3 | 30~300 | ||
8 | y=513.2x-154.1 | 0.992 4 | y=645.2x-94.2 | 0.999 | y=489.6 x-24.9 | 0.992 2 | 30~300 | ||
9 | y=168.6x + 97.5 | 0.998 6 | y=659.7x-1 236.2 | 0.992 4 | y=11 206.7x+103.1 | 0.991 4 | 10~200 | ||
10 | y=516.3x+323.1 | 0.996 4 | y=37 761.6x-16 018.5 | 0.994 3 | y=2 838.9x-117.9 | 0.997 2 | 10~200 | ||
11 | y=5 401.0x-7 552.3 | 0.999 4 | y=4 165.1x-131.9 | 0.992 4 | y=2 284.6x-9.43 | 0.992 4 | 30~300 | ||
12 | y=1 070.3x-1 143.6 | 0.998 7 | y=7 023.1x-24 364.7 | 0.992 7 | y=30 225.8x-1 013.4 | 0.991 8 | 40~400 | ||
13 | y=1 416.5x-255.8 | 0.998 1 | y=599.91x-2 183.1 | 0.991 4 | y=1 422.1x-12.0 | 0.994 2 | 10~200 | ||
14 | y=1 444.1x-2641.7 | 0.999 3 | y=8 233.9x-2 711.6 | 0.991 1 | y=3 181.0x-80.9 | 0.991 3 | 10~200 | ||
15 | y=218.4x-44.0 | 0.994 4 | y=224.9x-13.7 | 0.998 7 | y=933.3x-32.3 | 0.993 1 | 10~200 | ||
16 | y=1 674.7x-1 079.3 | 0.999 2 | y=18 059.6x-66 469.6 | 0.993 3 | y=4 552.4x+136.8 | 0.994 3 | 40~400 | ||
17 | y=1 911.6x-1 633.7 | 0.998 7 | y=1 599.6x+655.6 | 0.995 4 | y=2 427.1x-72.5 | 0.999 4 | 10~200 |
Tab. 3
Average recoveries, precisions and limits of quantifications of 17 cephalosporins"
序号 | 添加水平/(ng/g) | 水剂 | 油剂 | 膏霜类 | 定量限/(ng/g) | |||||
---|---|---|---|---|---|---|---|---|---|---|
平均回收率/% | RSD/% | 平均回收率/% | RSD/% | 平均回收率/% | RSD/% | |||||
1 | 10 | 98.85 | 1.00 | 94.78 | 5.77 | 103.20 | 1.26 | 10 | ||
20 | 98.57 | 3.71 | 92.64 | 5.22 | 99.60 | 1.29 | ||||
50 | 97.48 | 3.47 | 81.73 | 1.66 | 101.89 | 0.36 | ||||
2 | 10 | 88.73 | 8.85 | 80.90 | 1.30 | 108.56 | 1.37 | 10 | ||
20 | 103.66 | 5.38 | 79.68 | 7.73 | 100.19 | 0.92 | ||||
50 | 106.24 | 7.97 | 84.23 | 1.02 | 99.76 | 0.44 | ||||
3 | 10 | 90.92 | 4.28 | 100.67 | 3.95 | 100.85 | 1.27 | 10 | ||
20 | 93.44 | 9.11 | 84.81 | 5.29 | 91.35 | 0.68 | ||||
50 | 107.43 | 3.93 | 84.87 | 5.18 | 97.99 | 1.07 | ||||
4 | 30 | 100.60 | 7.55 | 86.68 | 6.98 | 102.85 | 0.48 | 30 | ||
60 | 96.31 | 4.69 | 87.89 | 2.51 | 104.07 | 0.71 | ||||
150 | 92.20 | 5.27 | 86.42 | 2.44 | 103.32 | 0.84 | ||||
5 | 30 | 91.33 | 7.56 | 101.77 | 5.64 | 109.32 | 0.37 | 30 | ||
60 | 79.84 | 10.00 | 88.56 | 9.51 | 108.20 | 1.25 | ||||
150 | 85.37 | 5.22 | 83.54 | 3.04 | 99.11 | 0.70 | ||||
6 | 10 | 109.93 | 5.36 | 93.78 | 8.98 | 99.46 | 0.83 | 10 | ||
20 | 107.58 | 8.68 | 85.05 | 5.59 | 102.52 | 0.80 | ||||
50 | 104.06 | 3.27 | 88.62 | 8.42 | 98.87 | 0.75 | ||||
7 | 30 | 99.43 | 9.68 | 84.00 | 8.39 | 84.15 | 0.79 | 30 | ||
60 | 109.19 | 3.00 | 77.92 | 5.16 | 91.49 | 2.71 | ||||
150 | 100.18 | 8.60 | 83.76 | 8.82 | 97.74 | 0.69 | ||||
8 | 30 | 90.39 | 3.37 | 92.91 | 8.19 | 84.85 | 0.72 | 30 | ||
60 | 86.41 | 5.69 | 79.40 | 6.49 | 99.41 | 1.21 | ||||
150 | 87.88 | 6.41 | 96.35 | 6.04 | 102.61 | 0.61 | ||||
9 | 10 | 80.60 | 9.69 | 89.07 | 1.55 | 106.00 | 1.87 | 10 | ||
20 | 79.33 | 8.96 | 94.02 | 5.23 | 103.42 | 0.69 | ||||
50 | 76.75 | 6.75 | 84.20 | 2.28 | 102.99 | 0.90 | ||||
10 | 10 | 99.80 | 7.73 | 106.12 | 6.25 | 94.64 | 1.75 | 10 | ||
20 | 109.73 | 4.29 | 88.70 | 8.09 | 89.53 | 0.86 | ||||
50 | 105.48 | 9.43 | 81.06 | 8.82 | 80.52 | 2.39 | ||||
11 | 30 | 84.79 | 7.81 | 75.27 | 1.59 | 105.06 | 9.57 | 30 | ||
60 | 80.06 | 9.72 | 76.05 | 1.28 | 106.05 | 4.82 | ||||
150 | 79.64 | 7.85 | 86.00 | 0.67 | 102.73 | 3.45 | ||||
12 | 40 | 104.68 | 6.70 | 84.05 | 2.60 | 109.83 | 6.15 | 40 | ||
80 | 100.70 | 8.36 | 107.67 | 3.88 | 105.40 | 1.02 | ||||
200 | 101.58 | 8.14 | 98.63 | 7.09 | 82.01 | 1.50 | ||||
13 | 10 | 81.59 | 7.32 | 81.57 | 5.33 | 99.35 | 0.95 | 10 | ||
20 | 80.63 | 1.25 | 90.37 | 9.37 | 101.84 | 0.71 | ||||
50 | 80.45 | 9.46 | 93.25 | 4.62 | 109.83 | 0.64 | ||||
14 | 10 | 80.46 | 8.44 | 90.52 | 5.84 | 87.60 | 1.39 | 10 | ||
20 | 98.13 | 7.16 | 98.71 | 6.80 | 96.23 | 0.50 | ||||
50 | 83.41 | 4.77 | 90.41 | 8.04 | 99.11 | 1.86 | ||||
15 | 10 | 95.71 | 3.78 | 106.2 | 2.59 | 108.20 | 4.77 | 10 | ||
20 | 83.84 | 3.76 | 104.30 | 0.57 | 110.32 | 0.93 | ||||
50 | 87.67 | 4.10 | 103.40 | 9.0 | 108.53 | 1.11 | ||||
16 | 40 | 80.33 | 9.26 | 84.20 | 1.86 | 103.18 | 0.55 | 40 | ||
80 | 94.91 | 8.28 | 82.52 | 4.83 | 104.05 | 1.24 | ||||
200 | 85.29 | 5.91 | 90.07 | 9.40 | 98.91 | 0.92 | ||||
17 | 10 | 106.44 | 3.14 | 83.27 | 2.21 | 92.97 | 1.23 | 10 | ||
20 | 100.20 | 4.57 | 84.53 | 6.43 | 80.07 | 1.26 | ||||
50 | 101.28 | 3.32 | 82.90 | 2.55 | 92.22 | 0.47 |
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