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

Abstract

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

CLC Number:

TQ658

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.

Figures/Tables 7

Fig. 1

Tab. 1

Tab. 2

Tab. 3

Tab. 4

Tab. 5

Tab. 6

References 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	—

Determination of 16 kinds of anti-infective drugs in cosmetics by LC-MS/MS

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序号	组分名称	检出浓度/（μg·g^-1）	最低定量浓度/（μg·g^-1）
1	酮康唑	0.50	2.5
2	甲硝唑	0.05	0.25
3	二水土霉素	0.25	1.0
4	盐酸多西环素	0.25	1.0
5	咪康唑	0.10	0.50
6	林可霉素	0.10	0.50
7	硝酸益康唑	0.10	0.50
8	氟康唑	0.10	0.50
9	盐酸萘替芬	0.10	0.50
10	氯霉素	0.20	0.50
11	盐酸四环素	0.25	1.0
12	盐酸金霉素	0.25	1.0
13	克林霉素	0.10	0.50
14	灰黄霉素	0.10	0.50
15	联苯苄唑	0.10	0.50
16	克霉唑	0.10	0.50

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