China Surfactant Detergent & Cosmetics ›› 2023, Vol. 53 ›› Issue (2): 226-232.doi: 10.3969/j.issn.1001-1803.2023.02.014
• Analytical methods and testing • Previous Articles Next Articles
Zhang Yanping1,*(),Zhou Zongzhou1,Huang Wanfeng1,Chen Yihua1,Zhang Min2,He Zuomin1
Received:
2022-03-03
Revised:
2023-01-29
Online:
2023-02-22
Published:
2023-02-23
Contact:
*E-mail: CLC Number:
Zhang Yanping, Zhou Zongzhou, Huang Wanfeng, Chen Yihua, Zhang Min, He Zuomin. Determination of 16 coumarin compounds in commonly cosmetics plant extract raw materials by UPLC-MS/MS[J].China Surfactant Detergent & Cosmetics, 2023, 53(2): 226-232.
Tab. 1
Source, batch number, purity and other information of 16 coumarin reference materials"
序号 | 名称 | 来源 | 批号 | 纯度/% |
---|---|---|---|---|
1 | 香豆素 | Bepure | D0009958 | 99.9 |
2 | 7-羟基香豆素 | Chemservice | 7642400 | 99.5 |
3 | 补骨脂素 | Bepure | A0014475 | 99.6 |
4 | 7-甲基香豆素 | Bepure | E0019273 | 99.5 |
5 | 异补骨脂素 | Bepure | C0013514 | 99.8 |
6 | 8-甲氧基补骨脂素 | Bepure | D0016009 | 99.9 |
7 | 欧前胡素 | Bepure | B0014639 | 99.0 |
8 | 异欧前胡素 | Bepure | B0009737 | 99.2 |
9 | 6,7-二甲氧基香豆素 | Bepure | C0007144 | 99.7 |
10 | 新补骨脂异黄酮 | 中检院 | 520052-201401 | 99.6 |
11 | 补骨脂二氢黄酮 | 中检院 | 520053-201401 | 99.4 |
12 | 4-甲基-7-羟基香豆素 | CATO | 1018-RC-0004 | 100.0 |
13 | 4-甲基-7-乙氧基香豆素 | Bepure | E0026326 | 99.9 |
14 | 5-甲氧基补骨脂素 | Bepure | A0014497 | 99.6 |
15 | 2,4,8-三甲基补骨脂素 | Bepure | C0013508 | 99.0 |
16 | 环香豆素 | Dr.E | 1063029 | 99.0 |
Tab. 3
Mass spectrometric condition for monitoring of 16 coumarin compounds"
序号 | 名称 | 保留时间/min | 母离子(m/z) | 子离子(m/z) | 锥孔电压/V | 碰撞电压/V |
---|---|---|---|---|---|---|
1 | 香豆素 | 5.43 | 146.9 | 90.9* | 32 | 20 |
76.9 | 22 | |||||
2 | 7-甲基香豆素 | 8.35 | 160.9 | 104.9* | 34 | 20 |
90.8 | 20 | |||||
3 | 7-羟基香豆素 | 4.00 | 162.9 | 106.9 * | 34 | 22 |
76.8 | 28 | |||||
4 | 4-甲基-7-羟基香豆素 | 4.76 | 176.9 | 120.9* | 38 | 22 |
104.9 | 20 | |||||
5 | 补骨脂素 | 8.21 | 186.9 | 130.9* | 34 | 26 |
76.8 | 36 | |||||
6 | 异补骨脂素 | 8.47 | 186.9 | 130.8* | 34 | 22 |
76.9 | 34 | |||||
7 | 4-甲基-7-乙氧基香豆素 | 9.20 | 205.0 | 176.9* | 32 | 20 |
104.9 | 22 | |||||
8 | 6,7-二甲氧基香豆素 | 5.06 | 207.0 | 106.9* | 36 | 34 |
150.9 | 22 | |||||
9 | 8-甲氧基补骨脂素 | 8.54 | 217.0 | 201.9* | 36 | 22 |
89.5 | 36 | |||||
10 | 5-甲氧基补骨脂素 | 8.92 | 217.0 | 202.0* | 34 | 24 |
117.9 | 32 | |||||
11 | 2,4,8-三甲基补骨脂素 | 9.73 | 229.1 | 141.8* | 42 | 24 |
173.0 | 22 | |||||
12 | 异欧前胡素 | 10.14 | 271.1 | 203.0* | 16 | 12 |
90.8 | 40 | |||||
13 | 欧前胡素 | 9.79 | 271.1 | 146.9* | 18 | 34 |
202.9 | 12 | |||||
14 | 环香豆素 | 10.44 | 323.2 | 120.9* | 24 | 44 |
251.0 | 18 | |||||
15 | 新补骨脂异黄酮 | 9.35 | 323.2 | 267.0* | 32 | 18 |
255.0 | 20 | |||||
16 | 补骨脂二氢黄酮 | 9.47 | 325.2 | 64.8* | 34 | 44 |
148.9 | 24 |
Tab. 4
Regression equation, correlation coefficient and limits of detection of 16 coumarin compounds"
序号 | 名称 | 线性范围/(μg/mL) | 回归方程 | 相关系数r | LOD/(μg/kg) | LOQ/(μg/kg) |
---|---|---|---|---|---|---|
1 | 香豆素 | 0.20~4.0 | Y=16 241.9X+104.8 | 0.998 8 | 18.0 | 60.0 |
2 | 7-羟基香豆素 | 0.10~2.0 | Y=45 779.9X-236.9 | 0.997 8 | 13.0 | 43.0 |
3 | 补骨脂素 | 0.10~2.0 | Y=99 642.9X+561.4 | 0.999 4 | 28.0 | 93.0 |
4 | 7-甲基香豆素 | 0.10~2.0 | Y=77 821.3X+452.9 | 0.998 1 | 23.0 | 77.0 |
5 | 异补骨脂素 | 0.10~2.0 | Y=100 678X+231.7 | 0.999 4 | 27.0 | 90.0 |
6 | 8-甲氧基补骨脂素 | 0.10~2.0 | Y=145 635X+298.1 | 0.999 5 | 10.0 | 33.0 |
7 | 欧前胡素 | 0.02~0.40 | Y=172 310X+431.8 | 0.999 2 | 3.0 | 10.0 |
8 | 异欧前胡素 | 0.02~0.40 | Y=81 886.4X+326.1 | 0.996 1 | 1.0 | 3.3 |
9 | 6,7-二甲氧基香豆素 | 0.02~0.40 | Y=108 121X-542.3 | 0.998 0 | 1.0 | 3.3 |
10 | 新补骨脂异黄酮 | 0.02~0.40 | Y=205 241X+412.6 | 0.999 8 | 0.7 | 2.2 |
11 | 补骨脂二氢黄酮 | 0.02~0.40 | Y=136 484X-326.1 | 0.997 5 | 1.3 | 4.5 |
12 | 4-甲基-7-羟基香豆素 | 0.01~0.20 | Y=47 302.3X+103.7 | 0.999 5 | 0.6 | 2.0 |
13 | 4-甲基-7-乙氧基香豆素 | 0.01~0.20 | Y=527 688X+523.9 | 0.998 9 | 0.7 | 2.2 |
14 | 5-甲氧基补骨脂素 | 0.01~0.20 | Y=388 853X-239.4 | 0.998 7 | 0.8 | 2.8 |
15 | 2,4,8-三甲基补骨脂素 | 0.01~0.20 | Y=493 485X+329.5 | 0.998 4 | 0.3 | 1.0 |
16 | 环香豆素 | 0.01~0.20 | Y=738 339X-204.2 | 0.998 6 | 0.6 | 2.0 |
Tab. 5
Results of recovery tests (n=6)for 16 coumarins compounds"
化合物 | 理论含量/μg | 平均回收率/% | RSD/% | ||||||||
---|---|---|---|---|---|---|---|---|---|---|---|
低 | 中 | 高 | 低 | 中 | 高 | 低 | 中 | 高 | |||
香豆素 | 4.25 | 8.49 | 16.98 | 85.7 | 90.3 | 91.4 | 4.6 | 3.9 | 5.1 | ||
7-羟基香豆素 | 2.12 | 4.23 | 8.46 | 91.6 | 95.7 | 92.7 | 2.8 | 3.8 | 3.1 | ||
补骨脂素 | 2.22 | 4.44 | 8.88 | 90.4 | 92.1 | 94.7 | 5.8 | 4.3 | 1.9 | ||
7-甲基香豆素 | 2.20 | 4.40 | 8.80 | 88.4 | 89.4 | 101.5 | 2.8 | 3.7 | 4.2 | ||
异补骨脂素 | 2.18 | 4.36 | 8.71 | 96.1 | 95.8 | 99.7 | 2.9 | 4.1 | 2.0 | ||
8-甲氧基补骨脂素 | 2.09 | 4.18 | 8.37 | 86.7 | 88.9 | 93.5 | 2.4 | 2.8 | 1.7 | ||
欧前胡素 | 0.43 | 0.85 | 1.71 | 92.7 | 95.7 | 102.8 | 4.8 | 3.5 | 2.8 | ||
异欧前胡素 | 0.42 | 0.83 | 1.66 | 96.8 | 94.7 | 98.3 | 4.5 | 3.8 | 3.5 | ||
6,7-二甲氧基香豆素 | 0.42 | 0.84 | 1.68 | 87.4 | 90.8 | 98.5 | 3.6 | 2.9 | 3.4 | ||
新补骨脂异黄酮 | 0.42 | 0.84 | 1.67 | 93.4 | 91.5 | 96.2 | 4.7 | 3.7 | 2.8 | ||
补骨脂二氢黄酮 | 0.44 | 0.88 | 1.76 | 94.8 | 96.4 | 108.6 | 3.4 | 3.5 | 3.0 | ||
4-甲基-7-羟基香豆素 | 0.22 | 0.45 | 0.90 | 89.6 | 92.8 | 102.3 | 2.9 | 3.7 | 1.5 | ||
4-甲基-7-乙氧基香豆素 | 0.22 | 0.45 | 0.90 | 98.4 | 101.5 | 99.7 | 5.3 | 3.7 | 3.8 | ||
5-甲氧基补骨脂素 | 0.21 | 0.42 | 0.84 | 86.9 | 95.1 | 98.5 | 4.5 | 3.8 | 2.9 | ||
2,4,8-三甲基补骨脂素 | 0.20 | 0.41 | 0.81 | 92.8 | 102.7 | 101.4 | 4.7 | 3.2 | 2.4 | ||
环香豆素 | 0.20 | 0.40 | 0.81 | 92.4 | 96.5 | 98.1 | 5.4 | 3.7 | 3.0 |
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