液质联用法测定化妆品中16种抗感染类药物

doi:10.3969/j.issn.1001-1803.2021.08.016

摘要/Abstract

摘要：

建立了采用液质联用法（liquid chromatography-tandem mass spectrometry, LC-MS/MS）检测化妆品中氟康唑等16种抗感染类药物的方法。结果表明,酮康唑线性范围为0.50~25 μg/g,其余15种线性范围为0.10~5.0 μg/g,相关系数r均大于0.99;精密度试验RSD均小于1.8%;酮康唑检出质量浓度为25 ng/mL,其余15种组分检出质量浓度均小于10 ng/mL;回收率试验结果在86.0%~112.4%范围之内。说明本方法具有良好的线性、精密度和回收率,适用于化妆品中氟康唑等16种抗感染类药物的检测。本方法结合国标方法,增加了8种组分的检测,加强了化妆品的监管力度,降低了化妆品的安全风险。

关键词: 液相色谱-串联质谱法, 化妆品, 抗感染类药物

Abstract:

A method based on liquid chromatography tandem mass spectrometry （LC-MS/MS） was established for the determination of 16 kinds of anti-infective drugs in cosmetics. The linear range of ketoconazole is 0.50-25 μg/g, and the linear range of the other 15 components is between 0.10-5.0 μg/g. The correlation coefficients are all greater than 0.99, and the RSD of precision test is less than 1.8%. The detection mass concentration of ketoconazole is 25 ng/mL, and the detection mass concentrations of the other 15 components are less than 10 ng/mL. The recoveries are in the range of 86.0%-112.4%. The method has good linearity, precision and recovery. It is suitable for the detection of 16 kinds of anti-infective drugs in cosmetics. Combined with the national standard method, this method adds the detection of 8 components, strengthens the supervision of cosmetics and reduces the safety risk of cosmetics.

Key words: LC-MS/MS, cosmetic, anti-infective drugs

中图分类号:

TQ658

沙丽娜,杨光勇,穆晓娟,张明玥. 液质联用法测定化妆品中16种抗感染类药物[J]. 日用化学工业, 2021, 51(8): 802-808.

Sha Lina,Yang Guangyong,Mu Xiaojuan,Zhang Mingyue. Determination of 16 kinds of anti-infective drugs in cosmetics by LC-MS/MS[J]. China Surfactant Detergent & Cosmetics, 2021, 51(8): 802-808.

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参考文献 13

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时间/min	V（A）/%	V（B）/%
0	85	15
1.0	85	15
2.0	55	45
4.0	40	60
4.8	20	80
5.0	85	15
9.0	85	15

序号	组分名称	母离子	子离子	锥孔电压/V	碰撞能/V
1	酮康唑	531.0	167.0	50	35
1	酮康唑	531.0	*255.0	50	35
2	甲硝唑	172.2	111.2	20	20
2	甲硝唑	172.2	*128.2	25	12
3	二水土霉素	461.4	201.2	40	20
3	二水土霉素	461.4	*426.4	40	18
4	盐酸多西环素	445.3	73.2	18	48
4	盐酸多西环素	445.3	*428.4	15	18
5	咪康唑	417.0	159.0	30	40
5	咪康唑	417.0	*161.0	30	35
6	林可霉素	407.2	*126.1	30	24
6	林可霉素	407.2	359.0	30	24
7	硝酸益康唑	381.0	*125.0	38	40
7	硝酸益康唑	381.0	193.0	38	35
8	氟康唑	307.0	*220.0	23	20
8	氟康唑	307.0	238.0	23	20
9	盐酸萘替芬	288.0	*117.0	21	22
9	盐酸萘替芬	288.0	141.0	21	20
10	氯霉素	323.2	165.2	22	25
10	氯霉素	323.2	*275.2	22	12
11	盐酸四环素	445.3	154.2	15	28
11	盐酸四环素	445.3	*410.2	10	16
12	盐酸金霉素	479.3	154.2	18	28
12	盐酸金霉素	479.3	*444.3	18	20
13	克林霉素	425.2	*126.4	30	25
13	克林霉素	425.2	377.5	18	16
14	灰黄霉素	353.0	*165.0	34	20
14	灰黄霉素	353.0	215.0	34	25
15	联苯苄唑	311.0	165.0	18	20
15	联苯苄唑	311.0	*243.0	18	17
16	克霉唑	277.0	*165.0	42	25
16	克霉唑	277.0	241.0	42	30

序号	组分名称	线性范围/（μg·g^-1）	回归方程	相关系数R
1	酮康唑	1.0 ~25	Y=13.988 3x-54.979 8	0.998 5
2	甲硝唑	0.10~5.0	Y=3 993.48x+179.122	0.999 7
3	二水土霉素	0.10~5.0	Y=86.491 8x-373.200	0.996 2
4	盐酸多西环素	0.10~5.0	Y=2 314.83x+140.865	0.999 7
5	咪康唑	0.10~5.0	Y=4 131.05x+476.666	0.999 2
6	林可霉素	0.10~5.0	Y=10 496.0x-120.741	0.998 3
7	硝酸益康唑	0.10~5.0	Y=7 639.27x-972.832	0.999 3
8	氟康唑	0.10~5.0	Y=663.417x-34.035 1	0.998 6
9	盐酸萘替芬	0.10~5.0	Y=4 606.00x+798.058	0.995 9
10	氯霉素	0.10~5.0	Y=87.988 3x-7.634 49	0.996 3
11	盐酸四环素	0.10~5.0	Y=1 340.38x-278.985	0.999 1
12	盐酸金霉素	0.10~5.0	Y=592.679x-37.470 0	0.997 8
13	克林霉素	0.10~5.0	Y=9 774.48x+923.635	0.999 7
14	灰黄霉素	0.10~5.0	Y=508.345x+46.885 1	0.994 1
15	联苯苄唑	0.10~5.0	Y=4 118.68x+578.258	0.999 4
16	克霉唑	0.10~5.0	Y=1 272.75x+20.350 5	0.999 4

序号	组分名称	加入质量浓度/（ng·mL^-1）	测得平均质量浓度/（ng·mL^-1）	回收率均值/%	RSD/%
1	酮康唑	8.679 6	8.754 8	101.0	2.69
2	甲硝唑	2.030 3	1.744 5	86.00	2.33
3	二水土霉素	1.773 7	1.740 0	98.20	3.21
4	盐酸多西环素	1.906 7	1.910 0	100.3	3.92
5	咪康唑	1.854 6	1.835 3	99.10	5.12
6	林可霉素	1.540 0	1.328 5	86.40	1.03
7	硝酸益康唑	1.814 4	1.824 8	100.7	1.75
8	氟康唑	1.794 8	1.800 9	100.5	1.83
9	盐酸萘替芬	2.039 7	2.026 9	99.50	7.38
10	氯霉素	1.926 9	2.100 6	109.2	2.95
11	盐酸四环素	2.091 2	2.057 0	98.50	4.05
12	盐酸金霉素	1.753 1	1.892 1	108.1	4.00
13	克林霉素	1.524 9	1.712 3	112.4	2.08
14	灰黄霉素	1.652 3	1.630 0	98.80	4.58
15	联苯苄唑	1.537 5	1.554 5	101.2	5.26
16	克霉唑	1.943 1	2.013 8	103.8	6.07

样品序号	含量/（μg·g^-1）
样品序号	氯霉素	甲硝唑	林可霉素	克林霉素
1号样	740.5	—	—	—
2号样	137.7	773.7	—	939.2
3号样	—	173.3	50.3	—