China Surfactant Detergent & Cosmetics ›› 2022, Vol. 52 ›› Issue (7): 785-790.doi: 10.3969/j.issn.1001-1803.2022.07.015
• Analytical methods and testing • Previous Articles Next Articles
Jiang Yaqi1,Gao Tianyang1,Yu Haiying1,Li Qiyan1,*(),Li Jun1,*(
),Xie Yaping2
Received:
2021-11-02
Revised:
2022-06-29
Online:
2022-07-22
Published:
2022-07-21
Contact:
Qiyan Li,Jun Li
E-mail:15253118118@163.com;13573756821@163.com
CLC Number:
Jiang Yaqi,Gao Tianyang,Yu Haiying,Li Qiyan,Li Jun,Xie Yaping. Rapid screening and determination of eight nitrosamines in cosmetics by liquid chromatography-quadrupole-time-of-flight mass spectrometry[J].China Surfactant Detergent & Cosmetics, 2022, 52(7): 785-790.
Tab. 1
Mass spectra of 8 nitrosamines"
序号 | 化合物名称 | 分子式 | 理论质量数(m/z) | 测得质量数(m/z) | 质量数偏差/ 10-6 | 主要碎片离子(m/z) |
---|---|---|---|---|---|---|
1 | N-亚硝基二甲胺(NDMA) | C2H6N2O | 75.055 | 75.055 3 | -0.5 | 43.028 4,44.049 2,58.052 3 |
2 | N-亚硝基二乙胺(NDEA) | C4H10N2O | 103.087 | 103.086 7 | 1.4 | 47.023 4,41.001 8,31.989 0 |
3 | N-亚硝基二丙胺(NDPA) | C6H14N2O | 131.118 | 131.118 3 | 2.8 | 41.037 7,39.022 2,43.053 4 |
4 | N-亚硝基二丁胺(NDBA) | C8H18N2O | 159.149 | 159.149 3 | 0.8 | 41.037 7,39.022 2,57.069 0 |
5 | N-亚硝基哌啶烷(NPIP) | C5H10N2O | 115.087 | 115.086 9 | 2.3 | 41.037 8,39.022 2,69.069 1 |
6 | N-亚硝基吗啉(NMOR) | C4H8N2O2 | 117.066 | 117.066 3 | 3.8 | 45.033 0,43.017 5,86.059 8 |
7 | N-亚硝基甲乙胺(NMEA) | C3H8N2O | 89.071 | 89.071 0 | 1.0 | 43.028 5,61.038 9,44.036 5 |
8 | N-亚硝基吡咯烷(NPYR) | C4H8N2O | 101.071 | 101.071 0 | 0.3 | 41.038 0,39.022 3,55.053 4 |
Tab. 2
Regression equations, linear range, LODs and LOQs of 8 nitrosamines"
化合物 | 回归方程 | 相关系数(r) | 线性范围/(ng/mL) | 检出限/(mg/kg) | 定量限/(mg/kg) |
---|---|---|---|---|---|
NDMA | y=6 186x-8 038 | 0.999 8 | 5~100 | 0.020 0 | 0.060 0 |
NDEA | y=4 783x-6 947 | 0.999 9 | 5~100 | 0.005 0 | 0.015 0 |
NDPA | y=2 303x-10 729 | 0.999 7 | 5~100 | 0.005 0 | 0.015 0 |
NDBA | y=1 352x-5 067 | 0.999 5 | 5~100 | 0.005 0 | 0.015 0 |
NPIP | y=5 959x-11 130 | 0.999 9 | 5~100 | 0.010 0 | 0.030 0 |
NMOR | y=2 746x-4 800 | 0.999 5 | 5~100 | 0.020 0 | 0.060 0 |
NMEA | y=4 334x-2 935 | 0.999 8 | 5~100 | 0.001 0 | 0.003 0 |
NPYR | y=5 034x-6 852 | 0.999 6 | 5~100 | 0.010 0 | 0.030 0 |
Tab. 3
Matrix effects for 8 nitrosamines"
化合物名称 | 基质效应/% | |||
---|---|---|---|---|
水剂 | 乳液 | 膏霜 | 粉饼 | |
NDMA | 113.2 | 112.6 | 123.5 | 110.5 |
NDEA | 108.3 | 106.3 | 116.5 | 102.5 |
NDPA | 117.2 | 96.0 | 122.7 | 110.7 |
NDBA | 123.5 | 104.8 | 127.7 | 116.2 |
NPIP | 105.9 | 114.9 | 121.2 | 104.9 |
NMOR | 124.4 | 99.2 | 129.1 | 109.5 |
NMEA | 112.1 | 117.5 | 130.0 | 107.5 |
NPYR | 120.0 | 119.5 | 127.3 | 110.7 |
Tab. 4
Recoveries of 8 nitrosamines in lotion, cream, emulsion and powder matrixes (n=6)"
化妆品基质 | 添加水平/(mg/kg) | 回收率(RSD)/% | |||||||
---|---|---|---|---|---|---|---|---|---|
NDMA | NMEA | NPYR | NPIP | NMOR | NDEA | NDPA | NDBA | ||
水剂 | 0.03 | 87.4(4.3) | 87.3(5.6) | 91.5(5.2) | 89.2(6.6) | 86.4(4.1) | 88.0(4.8) | 88.5(4.6) | 91.4(3.9) |
0.10 | 86.2(5.2) | 87.5(4.2) | 93.6(4.9) | 88.0(5.3) | 89.7(4.7) | 87.2(5.9) | 87.3(5.6) | 90.1(4.1) | |
0.50 | 104.5(3.6) | 101.7(5.0) | 112.8(3.2) | 108.4(4.8) | 109.3(2.6) | 100.3(4.2) | 99.4(2.7) | 111.3(5.2) | |
乳液 | 0.03 | 85.7(6.0) | 85.1(6.4) | 90.2(6.2) | 86.3(5.6) | 85.8(4.7) | 89.2(4.7) | 86.7(5.5) | 87.9(3.8) |
0.10 | 86.6(6.5) | 87.1(6.0) | 91.4(5.2) | 89.5(4.6) | 89.8(5.0) | 88.6(5.7) | 88.7(4.6) | 89.9(4.8) | |
0.50 | 97.2(4.4) | 102.2(3.6) | 108.5(4.5) | 110.3(3.2) | 112.7(1.4) | 103.3(5.6) | 106.4(1.5) | 113.1(2.2) | |
膏霜 | 0.03 | 85.8(4.5) | 88.5(5.5) | 92.4(5.3) | 86.5(4.2) | 89.5(6.4) | 87.4(6.0) | 86.8(5.3) | 91.4(4.8) |
0.10 | 85.6(6.6) | 86.3(6.5) | 90.6(3.7) | 87.5(5.4) | 88.2(5.2) | 86.9(6.1) | 87.8(4.7) | 90.2(3.5) | |
0.50 | 95.7(4.5) | 98.4(4.8) | 110.5(1.8) | 107.6(3.5) | 110.6(3.3) | 98.7(5.2) | 103.9(3.8) | 107.1(3.0) | |
粉饼 | 0.03 | 88.7(5.8) | 89.2(4.7) | 90.5(5.1) | 86.1(6.1) | 88.4(4.8) | 88.6(4.3) | 87.9(5.6) | 87.3(5.9) |
0.10 | 85.1(6.3) | 87.4(4.4) | 92.8(3.1) | 89.1(6.2) | 87.5(5.2) | 86.9(5.7) | 88.4(5.2) | 88.4(4.8) | |
0.50 | 97.4(3.4) | 93.2(6.1) | 109.4(3.0) | 104.1(3.9) | 101.0(4.7) | 90.5(5.2) | 95.6(3.9) | 107.2(4.8) |
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