高效液相色谱法测定化妆品中22种防晒剂

doi:10.3969/j.issn.1001-1803.2021.06.015

Abstract

Abstract:

A high performance liquid chromatography （HPLC） method was established for the determination of 22 sunscreens in cosmetics. The samples were extracted, ultrasonicated and then filtered. The target compounds were separated by OSAKA SODA CAPCELL PAK C₁₈ MGⅡcolumn, and analyzed by HPLC with PDA detector. Under the optimized experimental conditions, there is a good linear relationship between peaks areas and sunscreens concentrations with the r values are higher than 0.999. The detection limits are in the range of 0.01%-0.11%, and the limits of quantification are in the range of 0.03%-0.34%. The average recoveries are in the range of 89.7%-109.8% with the relative standard deviations are less than 5%. This accurate and sensitive method is suitable for the qualitative and quantitative analysis of 22 sunscreens in cosmetics.

Key words: cosmetics, sunscreen, high performance liquid chromatography

CLC Number:

TQ658

HAN Wei,LIU Jie,LI Li-xia,LV Xiao-jun. Determination of 22 sunscreens by high performance liquid chromatography in cosmetics[J].China Surfactant Detergent & Cosmetics, 2021, 51(6): 569-576.

Figures/Tables 12

Tab. 1

Tab. 2

Tab. 3

Fig. 1

Fig. 2

Fig. 3

Fig. 4

Tab. 4

Fig. 5

Tab. 5

Calibration curves, limits of detection and limits of quantification"

编号	防晒剂名称	回归方程	相关系数	线性范围/ （μg·mL^-1）			检出限/%	定量限/%
1	3-亚苄基樟脑	y=3.35×10⁴x-3.77×10³	0.999 9	1.36	~	17.04	0.01	0.05
2	4-甲基苄亚基樟脑	y=5.33×10⁴x-7.51×10³	1.000 0	2.17	~	27.17	0.02	0.09
3	二苯酮-3	y=2.53×10⁴x-3.55×10³	1.000 0	2.16	~	26.99	0.02	0.09
4	二苯酮-4或二苯酮-5	y=1.76×10⁴x-2.82×10³	0.999 9	2.31	~	28.82	0.02	0.09
5	亚苄基樟脑磺酸	y=3.50×10⁴x-4.28×10³	1.000 0	1.73	~	21.62	0.02	0.07
6	双-乙基己氧苯酚甲氧苯基三嗪	y=4.67×10⁴x-9.74×10³	0.999 7	2.08	~	26.04	0.03	0.08
7	丁基甲氧基二苯甲酰基甲烷	y=1.74×10⁴x-1.46×10⁴	1.000 0	2.73	~	34.15	0.03	0.11
8	樟脑苯扎铵甲基硫酸盐	y=1.02×10⁴x+1.82×10³	0.999 4	1.56	~	19.44	0.02	0.06
9	二乙氨羟苯甲酰基苯甲酸己酯	y=6.72×10³x-2.80×10³	0.999 9	4.48	~	55.95	0.06	0.18
10	二乙基己基丁酰胺基三嗪酮	y=9.50×10⁴x-3.47×10³	0.999 9	0.54	~	6.72	0.01	0.02
11	甲酚曲唑三硅氧烷	y=1.96×10⁴x-1.23×10³	0.999 8	1.45	~	18.13	0.02	0.06
12	二甲基PABA乙基己酯	y=6.19×10⁴x-8.67×10³	1.000 0	1.79	~	22.33	0.02	0.07
13	甲氧基肉桂酸乙基己酯	y=6.22×10⁴x-3.21×10⁴	0.999 9	1.93	~	24.11	0.02	0.08
14	水杨酸乙基己酯	y=1.17×10⁴x-1.62×10⁴	0.999 9	5.02	~	62.69	0.06	0.20
15	乙基己基三嗪酮	y=1.02×10⁵x-8.41×10³	0.999 9	1.09	~	13.67	0.01	0.04
16	胡莫柳酯	y=1.15×10⁴x-2.78×10⁴	0.999 9	8.58	~	107.29	0.11	0.34
17	对甲氧基肉桂酸异戊酯	y=6.02×10⁴x-4.34×10³	1.000 0	1.05	~	13.17	0.01	0.04
18	亚甲基双-苯并三唑基四甲基丁基酚	y=2.88×10⁴x-4.29×10³	0.999 7	0.91	~	11.43	0.01	0.04
19	奥克立林	y=3.57×10⁴x-2.68×10⁴	0.999 9	2.85	~	35.60	0.03	0.11
20	苯基苯并咪唑磺酸	y=3.67×10⁴x-9.47×10²	1.000 0	1.63	~	20.36	0.02	0.07
21	对苯二亚甲基二樟脑磺酸	y=7.32×10³x-1.92×10³	0.999 9	2.17	~	27.11	0.03	0.09
22	苯基二苯并咪唑四磺酸酯二钠	y=1.14×10⁴x-3.20×10³	0.999 6	2.62	~	32.79	0.01	0.03

Tab. 5

Tab. 6

Recoveries and precisions of 22 sunscreens spiked in cosmetic samples"

编号	防晒剂名称	添加量/μg	乳状		蜡状
编号	防晒剂名称	添加量/μg	平均回收率/%	RSD/%	平均回收率/%	RSD/%
1	3-亚苄基樟脑	511.2	109.3	1.06	107.2	0.99
		852.0	98.6	0.94	101.0	1.06
		1 704.0	101.5	0.83	103.2	1.03
2	4-甲基苄亚基樟脑	815.1	109.3	0.33	106.8	0.31
		1 358.5	98.4	0.56	99.7	0.58
		2 717.0	101.4	0.13	102.3	0.89
3	二苯酮-3	809.8	109.1	0.19	106.6	0.69
		1 349.7	98.1	0.59	98.8	0.91
		2 699.3	101.7	0.17	98.9	1.35
4	二苯酮-4或二苯酮-5	864.5	108.3	0.34	102.6	0.81
		1 440.8	99.7	0.57	100.1	1.03
		2 881.6	102.0	0.11	103.0	0.52
5	亚苄基樟脑磺酸	648.7	109.1	0.66	107.8	0.45
		1 081.2	98.5	0.28	96.8	0.69
		2 162.5	101.1	0.34	101.1	0.65
6	双-乙基己氧苯酚甲氧苯基三嗪	781.1	93.9	1.91	93.3	0.89
		1 301.9	94.9	0.41	95.8	0.43
		2 603.7	92.3	1.38	93.2	0.82
7	丁基甲氧基二苯甲酰基甲烷	1 024.5	106.9	0.31	104.0	1.05
		1 707.6	100.0	0.54	95.8	0.53
		3 415.2	90.2	0.32	94.2	1.33
8	樟脑苯扎铵甲基硫酸盐	466.6	97.2	0.25	91.7	1.28
		777.6	93.1	0.93	94.5	0.76
		1 555.3	94.7	0.67	96.4	0.56
9	二乙氨羟苯甲酰基苯甲酸己酯	1 678.5	108.6	0.52	105.7	0.52
		2 797.5	97.7	0.50	103.3	1.19
		5 594.9	101.7	0.49	102.5	0.26
10	二乙基己基丁酰胺基三嗪酮	201.5	108.8	1.96	98.7	1.39
		335.8	96.3	1.25	104.1	3.02
		671.7	99.1	1.05	96.1	2.11
11	甲酚曲唑三硅氧烷	543.9	92.8	1.18	94.0	3.06
		906.5	91.5	1.55	93.1	1.17
		1 813.1	91.9	0.61	91.5	1.27
12	二甲基PABA乙基己酯	669.9	109.8	0.16	103.2	0.77
		1 116.5	98.5	0.45	103.1	0.66
		2 233.0	101.3	0.22	106.0	0.84
13	甲氧基肉桂酸乙基己酯	723.4	107.2	0.31	103.8	0.35
		1 205.6	100.4	0.32	101.5	1.50
		2 411.2	89.8	0.22	101.9	0.79
14	水杨酸乙基己酯	1 880.7	105.8	0.54	97.5	0.99
		3 134.6	100.0	0.78	99.4	1.06
		6 269.2	90.1	1.52	103.5	1.24
15	乙基己基三嗪酮	410.1	92.8	0.71	92.9	1.64
		683.6	94.0	0.63	94.9	2.09
		1 367.1	93.2	0.86	99.7	0.75
16	胡莫柳酯	3 218.7	105.8	0.58	106.8	1.06
		5 364.5	99.8	0.84	101.9	0.58
		10 728.9	90.6	1.35	104.8	0.40
17	对甲氧基肉桂酸异戊酯	395.2	109.1	1.44	106.7	1.89
		658.7	98.0	0.40	108.5	2.50
		1 317.3	101.2	0.25	98.3	0.80
18	亚甲基双-苯并三唑基四甲基丁基酚	342.9	102.9	3.02	102.6	3.38
		571.4	101.9	1.87	102.0	2.41
		1 142.9	96.9	3.15	97.2	1.51
19	奥克立林	1 548.6	106.8	0.13	104.5	0.68
		2 581.0	100.5	0.43	103.0	0.62
		5 162.0	89.7	0.15	105.6	1.22
20	苯基苯并咪唑磺酸	488.6	107.1	1.27	93.4	3.07
		814.4	107.1	0.62	94.8	2.19
		1 628.8	104.3	0.39	93.8	1.28
21	对苯二亚甲基二樟脑磺酸	813.3	105.1	1.10	104.1	1.11
		1 355.5	100.2	1.17	105.7	3.24
		2 711.0	101.2	0.96	102.3	3.30
22	苯基二苯并咪唑四磺酸酯二钠	1 180.3	100.4	0.82	100.1	0.55
		1 967.2	98.6	0.15	99.6	0.65
		3 934.3	100.3	1.03	101.0	0.51

Tab. 6

Tab. 7

References 12

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组分	新标准提取试剂		本方法提取试剂
组分	非蜡状	蜡状	非蜡状	蜡状
Ⅰ组	混合溶剂1	四氢呋喃	混合溶剂1	混合溶剂1
Ⅱ组	混合溶剂1	四氢呋喃	四氢呋喃	四氢呋喃

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[9]	Zhen Xie, Wei Huang, Jinsong Zhang, Shuhuai Chen, Linji Qu, Rong Kuang. Study on biomarkers of corneal injury in the evaluation of eye irritation of cosmetics [J]. China Surfactant Detergent & Cosmetics, 2024, 54(2): 161-167.
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Determination of 22 sunscreens by high performance liquid chromatography in cosmetics

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编号	防晒剂名称	定容溶剂	分组
1	3-亚苄基樟脑	混合溶液1	Ⅰ组
2	4-甲基苄亚基樟脑	混合溶液1
3	二苯酮-3	混合溶液1
4	二苯酮-4或二苯酮 -5	混合溶液1
5	亚苄基樟脑磺酸	混合溶液1
7	丁基甲氧基二苯甲酰基甲烷	四氢呋喃
8	樟脑苯扎铵甲基硫酸盐	混合溶液
9	二乙氨羟苯甲酰基苯甲酸己酯	混合溶液1
10	二乙基己基丁酰胺基三嗪酮	混合溶液1
12	二甲基 PABA乙基己酯	混合溶液1
13	甲氧基肉桂酸乙基己酯	四氢呋喃
14	水杨酸乙基己酯	四氢呋喃
16	胡莫柳酯	四氢呋喃
17	对甲氧基肉桂酸异戊酯	混合溶液1
19	奥克立林（以酸计）	四氢呋喃
20	苯基苯并咪唑磺酸	混合溶液1
21	对苯二亚甲基二樟脑磺酸	混合溶液1
6	双-乙基己氧苯酚甲氧苯基三嗪	四氢呋喃	Ⅱ组
11	甲酚曲唑三硅氧烷	四氢呋喃
15	乙基己基三嗪酮	四氢呋喃
18	亚甲基双-苯并三唑基四甲基丁基酚	四氢呋喃
22	苯基二苯并咪唑四磺酸酯二钠	混合溶液2	Ⅲ组

t/min	φ（A）/%	φ（B）/%	φ（C）/%
0	18	2	80
4	6	25	69
8	30	30	40
16	20	45	35
20	20	45	35
22	45	35	20
26	45	35	20
27	45	45	10
40	45	45	10
41	18	2	80
46	18	2	80

编号	防晒剂名称	限值/%	含量检出范围/%	检出批数	检出率/%
1	3-亚苄基樟脑	2	0	0	0
2	4-甲基苄亚基樟脑	4	1.9~3.3	3	15
3	二苯酮-3	10	2.0~4.9	3	15
4	二苯酮-4或二苯酮-5	5（以酸计）	0	0	0
5	亚苄基樟脑磺酸	6（以酸计）	0	0	0
6	双-乙基己氧苯酚甲氧苯基三嗪	10	0.4~3.0	10	50
7	丁基甲氧基二苯甲酰基甲烷	5	0.3~2.9	8	40
8	樟脑苯扎铵甲基硫酸盐	6	0	0	0
9	二乙氨羟苯甲酰基苯甲酸己酯	10	0.5~4.0	9	45
10	二乙基己基丁酰胺基三嗪酮	10	0	0	0
11	甲酚曲唑三硅氧烷	15	0.8~2.5	3	15
12	二甲基PABA乙基己酯	8	0	0	0
13	甲氧基肉桂酸乙基己酯	10	2.0~8.7	17	85
14	水杨酸乙基己酯	5	3.8~4.6	8	40
15	乙基己基三嗪酮	5	2.8~4.3	4	20
16	胡莫柳酯	10	2.4~8.4	4	20
17	对甲氧基肉桂酸异戊酯	10	0	0	0
18	亚甲基双-苯并三唑基四甲基丁基酚	10	1.2~1.3	2	10
19	奥克立林	10（以酸计）	1.1~3.2	8	40
20	苯基苯并咪唑磺酸	8（以酸计）	2.0~3.8	6	30
21	对苯二亚甲基二樟脑磺酸	10（以酸计）	3.1	1	5
22	苯基二苯并咪唑四磺酸酯二钠	10（以酸计）	0	0	0

t/min	φ（A）/%	φ（B）/%	φ（C）/%
0	18	2	80
4	6	25	69
8	30	30	40
16	20	45	35
20	20	45	35
22	45	35	20
26	45	35	20
27	45	45	10
40	45	45	10
41	18	2	80
46	18	2	80

t/min	φ（A）/%	φ（B）/%	φ（C）/%
0	18	2	80
4	6	25	69
8	30	30	40
16	20	45	35
20	20	45	35
22	45	35	20
26	45	35	20
27	45	45	10
40	45	45	10
41	18	2	80
46	18	2	80