超高效液相色谱串联质谱法同时测定化妆品中94种非法添加化合物

doi:10.3969/j.issn.1001-1803.2020.07.011

Abstract

Abstract:

A method for simultaneous determination of 94 kinds of illegally added compounds in cosmetics by ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） was established. The cosmetic samples were extracted with the mixed solvent of 70% acetonitrile-water under ultrasonic assistance. Then the components in the purified extract were separated by CORTECS?UPLC?C₁₈ column （2.1 mm×100 mm, 1.6 μm） with 0.1% formic acid/acetonitrile solution-0.1% formic acid and 5 mmol/L ammonium acetate as mobile phase, and then detected by UPLC-MS/MS. The method showed that good linearity was obtained with correlation coefficients higher than 0.995. The range of the limit of quantitation for this method was 0.025-0.1 μg/g. The spiked recovery was in the range of 51.1%-129.3%, and the RSD was 1.8%-19.0%.

Key words: cosmetics, illegally added compound, ultra performance liquid chromatography-tandem mass spectrometry

CLC Number:

TQ658

WANG Tong-zhen,ZHENG Yu-li,LIANG Hai-yun,KE Li-qun,CAO Wei-qiang. Simultaneous determination of 94 kinds of illegally added compounds in cosmetics by ultra performance liquid chromatography-tandem mass spectrometry[J].China Surfactant Detergent & Cosmetics, 2020, 50(7): 496-503.

Figures/Tables 2

Tab. 1

MS/MS parameters for 94 kinds of compounds"

序号	化合物	m/z			碰撞能/V		锥孔电压/V	电离模式
序号	化合物	母离子	子离子	子离子	碰撞能/V		锥孔电压/V	电离模式
1	甲硝唑	172.0	82.0	128.0*	21	15	30	ESI+
2	磺胺吡啶	250.0	108.0	156.0*	25	16	33	ESI+
3	磺胺甲口恶唑	254.1	92.0*	156.0	25	15	30	ESI+
4	磺胺甲嘧啶	265.1	92.0*	156.0	25	15	35	ESI+
5	磺胺甲二唑	271.1	92.0*	156.0	25	15	30	ESI+
6	克霉唑	277.1	165.1*	241.0	24	20	10	ESI+
7	磺胺甲氧嗪	281.1	108.0	156.0*	20	15	35	ESI+
8	磺胺氯哒嗪	285.0	92.0*	156.0	28	15	35	ESI+
9	睾酮	289.2	97.1*	109.1	20	20	35	ESI+
10	甲基睾丸酮	303.2	97.0*	109.0	25	27	30	ESI+
11	氟康唑	307.1	220.1	238.1*	15	15	10	ESI+
12	孕三烯酮	309.0	199.0	241.1*	34	22	28	ESI+
13	联苯苄唑	311.2	165.0	243.1*	10	15	20	ESI+
14	炔诺孕酮	313.2	109.0*	245.1	26	18	30	ESI+
15	黄体酮	315.2	97.0*	109.0	22	24	30	ESI+
16	诺氟沙星	320.1	233.0*	276.1	25	20	40	ESI+
17	依诺沙星	321.1	234.1*	303.1	21	16	40	ESI+
18	呋喃它酮	325.2	252.2*	281.03	16	12	25	ESI+
19	环丙沙星	332.1	245.1	288.2*	22	16	40	ESI+
20	培氟沙星	334.1	290.1*	316.1	19	19	42	ESI+
21	螺内酯	341.2	91.1	107.1*	50	25	25	ESI+
22	灰黄霉素	353.2	165.0*	215.0	20	20	6	ESI+
23	泼尼松	359.2	147.2	341.2*	20	10	30	ESI+
24	恩诺沙星	360.3	316.3*	342.3	20	20	45	ESI+
25	泼尼松龙	361.1	147.0	343.1*	20	10	20	ESI+
26	可的松	361.3	121.1*	163.2	28	25	40	ESI+
27	氧氟沙星	362.3	261.3	318.3*	30	20	25	ESI+
28	氢化可的松	363.2	105.1	121.1*	35	25	35	ESI+
29	氟罗沙星	370.4	269.3	326.3*	25	20	30	ESI+
30	甲基泼尼松龙	375.1	161.1	357.1*	20	10	20	ESI+
31	氟米龙	377.2	279.2*	321.3	15	13	23	ESI+
32	异氟泼尼松	379.1	341.0*	359.0	10	10	30	ESI+
33	醋酸甲地孕酮	385.2	267.1*	325.1	18	15	30	ESI+
34	沙拉沙星	386.2	299.1	342.1*	27	18	45	ESI+
35	醋酸甲羟孕酮	387.2	123.0*	327.0	20	10	20	ESI+
36	倍他米松	393.3	147.2	355.2*	25	12	20	ESI+
37	地塞米松	393.3	147.3	355.3*	25	10	20	ESI+
38	曲安西龙	395.2	225.15	357.2*	18	11	20	ESI+
39	双氟沙星	400.3	356.2*	382.2	20	20	30	ESI+
40	泼尼松醋酸酯	401.25	147.1	295.2*	25	13	28	ESI+
41	莫西沙星	402.1	110.1*	358.1	25	18	50	ESI+
42	醋酸泼尼松龙	403.15	147.1	385.2*	18	8	20	ESI+
43	醋酸可的松	403.2	163.2*	343.2	25	28	35	ESI+
44	醋酸氯地孕酮	405.1	269.0	309.3*	18	18	30	ESI+
45	醋酸氢化可的松	405.25	121.05	309.2*	34	17	25	ESI+
46	林可霉素	407.2	126.1*	359.3	25	20	40	ESI+
47	倍氯米松	409.2	147.0	391.0*	25	12	25	ESI+
48	氟米松	411.25	121.1	253.15*	35	16	26	ESI+
49	地索奈德	417.1	225.1	323.2*	23	10	20	ESI+
50	甲基泼尼松龙醋酸酯	417.1	253.2	399.1*	20	10	20	ESI+
51	醋酸氟米龙	419.1	279.0*	321.0	10	10	20	ESI+
52	醋酸氟氢可的松	423.1	121.0*	239.0	30	39	40	ESI+
53	克林霉素	425.2	126.1*	377.2	45	28	30	ESI+
54	己酸羟孕酮	429.1	217.2	313.2*	16	13	20	ESI+
55	布地奈德	431.1	147.0	413.1*	30	10	20	ESI+
56	氢化可的松丁酸酯	433.3	121.1*	345.3	24	12	35	ESI+
57	醋酸倍他米松	435.1	309.0	337.0*	10	10	20	ESI+
58	氟尼缩松	435.2	321.2	397.1*	13	10	30	ESI+
59	地塞米松醋酸酯	435.25	309.2	337.2*	13	12	21	ESI+
60	曲安奈德	435.25	339.2	397.2*	13	13	20	ESI+
61	氟氢缩松	437.3	121.1	361.2*	31	16	40	ESI+
62	地夫可特	442.1	124.0	142.0*	50	35	20	ESI+
63	多西环素	445.0	154.1	428.1*	30	18	35	ESI+
64	卤米松	445.1	155.0*	287.1	30	10	20	ESI+
65	四环素	445.1	410.1*	427.1	18	12	30	ESI+
66	戊酸氢化可的松	447.1	121.0	345.1*	25	10	20	ESI+
67	氟轻松	453.3	121.0*	337.2	30	10	20	ESI+
68	哈西奈德	455.1	104.9	121.0*	40	30	40	ESI+
69	米诺环素	458.2	352.1	441.1*	30	19	36	ESI+
70	土霉素	461.0	426.1*	443.1	18	11	30	ESI+
71	氯倍他索丙酸酯	467.1	355.0	373.0*	10	10	20	ESI+
72	氯替泼诺	467.2	265.1*	359.1	15	10	20	ESI+
73	曲安奈德醋酸酯	477.1	321.0	339.0*	10	10	20	ESI+
74	倍他米松戊酸酯	447.4	279.0	355.0*	15	10	20	ESI+
75	金霉素	479.0	444.0*	462.1	20	15	35	ESI+
76	曲安西龙双醋酸酯	479.2	321.0	441.0*	15	10	20	ESI+
77	戊酸双氟可龙	479.2	375.3*	439.35	10	10	25	ESI+
78	丁酸氯倍他松	479.25	279.2	343.2*	16	14	35	ESI+
79	卤倍他索丙酸酯	485.2	353.15*	391.25	13	10	30	ESI+
80	泼尼卡酯	489.1	115.0*	381.0	20	10	20	ESI+
81	二氟拉松双醋酸酯	495.25	279.2	317.2*	14	13	26	ESI+
82	氟轻松醋酸酯	495.3	121.1*	337.0	40	15	22	ESI+
83	氟替卡松丙酸酯	501.2	293.2	313.2*	14	12	25	ESI+
84	安西奈德	503.2	321.2	339.2*	17	12	21	ESI+
85	倍他米松双丙酸酯	505.3	279.2*	319.2	16	14	24	ESI+
86	莫米他松糠酸酯	521.1	263.0	503.1*	20	10	20	ESI+
87	阿氯米松双丙酸酯	521.25	279.2	301.2*	14	16	24	ESI+
88	倍氯米松双丙酸酯	521.3	319.25	503.25*	15	10	25	ESI+
89	酮康唑	531.2	244.0	489.3*	30	28	26	ESI+
90	环索奈德	541.3	323.2	523.2*	20	10	30	ESI+
91	克拉霉素	748.6	158.1*	590.6	30	20	35	ESI+
92	阿奇霉素	749.5	158.2*	591.5	40	30	30	ESI+
93	罗红霉素	837.5	158.2*	679.5	32	20	40	ESI+
94	氯霉素	321.2	152.2	257.2*	15	10	-45	ESI-

Tab. 1

Tab. 2

Retention time, linear rang, linear equation, correlation coefficient, limit of quantitation and precision of 94 kinds of illegally added compounds"

序号	化合物	保留时间/min	线性范围/（μg·L^-1）	线性方程	相关系数	定量限/（μg·g^-1）	精密度/%	回收率/%
1	甲硝唑	0.96	0.5~400	Y=2 208.8X+930.1	0.995	0.025	9.6	51.7
2	磺胺吡啶	1.23	0.5~400	Y=2 645.0X+761.3	0.998	0.025	6.5	97.5
3	磺胺甲口恶唑	2.58	0.5~400	Y=2 463.5X+301.1	0.999	0.025	2.8	94.0
4	磺胺甲嘧啶	1.33	0.5~400	Y=4 347.4X+727.8	0.998	0.025	5.3	98.2
5	磺胺甲二唑	1.50	0.5~400	Y=1 874.9X+283.0	0.998	0.025	5.3	96.7
6	克霉唑	5.64	0.5~400	Y=12 647.5X+1 230.4	0.999	0.025	2.1	97.1
7	磺胺甲氧嗪	1.58	0.5~400	Y=4 361.3X+2 053.7	0.996	0.025	5.5	95.6
8	磺胺氯哒嗪	2.21	0.5~400	Y=1 830.4X+490.3	0.997	0.025	4.4	92.7
9	睾酮	5.81	0.5~400	Y=2 694.1X+486.4	0.999	0.025	5.0	88.6
10	甲基睾丸酮	6.25	0.5~400	Y=4 549.2X+821.5	0.998	0.025	3.1	87.8
11	氟康唑	1.68	0.5~400	Y=728.5X+82.7	0.998	0.025	6.1	88.2
12	孕三烯酮	6.12	0.5~400	Y=1 426.6X+90.3	0.997	0.025	3.7	83.5
13	联苯苄唑	5.65	0.5~400	Y=31 765.3X+4 326.9	0.998	0.025	1.8	97.3
14	炔诺孕酮	6.73	0.5~400	Y=690.6X+189.8	0.998	0.025	3.8	95.9
15	黄体酮	7.88	0.5~400	Y=2 074.6X+294.2	0.999	0.025	2.2	87.8
16	诺氟沙星	1.00	0.5~400	Y=1 776.6X+218.0	0.998	0.025	18.4	70.2
17	依诺沙星	0.95	0.5~400	Y=2 458.9X+120.4	0.999	0.025	16.5	73.0
18	呋喃它酮	1.02	0.5~400	Y=792.7X+261.2	0.997	0.025	7.8	84.8
19	环丙沙星	1.07	0.5~400	Y=2 794.9X+563.1	0.998	0.025	18.5	90.7
20	培氟沙星	1.05	0.5~400	Y=4 601.7X+1 088.3	0.996	0.025	12.8	98.9
21	螺内酯	6.53	0.5~400	Y=413.7X+21.5	0.999	0.025	2.5	103.1
22	灰黄霉素	5.49	0.5~400	Y=1 459.7X+295.4	0.999	0.025	2.8	99.8
23	泼尼松	3.80	0.5~400	Y=440.9X+243.1	0.996	0.025	5.0	97.9
24	恩诺沙星	1.27	0.5~400	Y=5 904.6X+52.9	0.999	0.025	11.4	102.2
25	泼尼松龙	3.79	0.5~400	Y=879.2X+510.2	0.995	0.025	3.0	99.1
26	可的松	3.80	0.5~400	Y=395.8X+204.9	0.995	0.025	3.8	100.4
27	氧氟沙星	1.03	0.5~400	Y=3 810.5X+486.5	0.997	0.025	11.7	89.6
28	氢化可的松	3.88	0.5~400	Y=398.6X+31.6	0.999	0.025	4.1	89.9
29	氟罗沙星	1.06	0.5~400	Y=3 271.1X+313.0	0.997	0.025	9.2	89.8
30	甲基泼尼松龙	4.47	0.5~400	Y=1 170.5X+470.8	0.997	0.025	5.2	93.6
31	氟米龙	5.32	0.5~400	Y=458.5X+15.4	0.998	0.025	6.1	99.5
32	异氟泼尼松	3.79	0.5~400	Y=491.2X+338.2	0.995	0.025	4.1	97.8
33	醋酸甲地孕酮	7.79	0.5~400	Y=1 316.8X+55.8	0.999	0.025	4.3	98.4
34	沙拉沙星	1.67	0.5~400	Y=2 755.7X-242.3	0.999	0.025	8.7	108.1
35	醋酸甲羟孕酮	8.02	0.5~400	Y=352.1X+56.0	0.999	0.025	5.9	92.4
36	倍他米松	4.63	0.5~400	Y=323.4X+68.8	0.998	0.025	4.8	101.0
37	地塞米松	4.56	0.5~400	Y=299.4X+56.3	0.996	0.025	4.0	102.5
38	曲安西龙	2.81	0.5~400	Y=161.7X+12.7	0.996	0.025	6.1	93.5
39	双氟沙星	1.80	0.5~400	Y=3 499.3X-623.5	0.999	0.025	4.9	102.9
40	泼尼松醋酸酯	5.45	0.5~400	Y=348.6X+13.5	0.999	0.025	6.1	104.5
41	莫西沙星	2.26	0.5~400	Y=1 140.1X-186.5	0.999	0.025	15.2	95.9
42	醋酸泼尼松龙	5.19	0.5~400	Y=944.2X+359.2	0.996	0.025	6.3	96.6
43	醋酸可的松	5.55	0.5~400	Y=325.4X+19.5	0.999	0.025	5.3	79.7
44	醋酸氯地孕酮	7.97	0.5~400	Y=206.7X-16.8	0.999	0.025	4.3	94.2
45	醋酸氢化可的松	5.30	0.5~400	Y=139.1X+53.2	0.997	0.025	5.7	70.2
46	林可霉素	0.87	0.5~400	Y=8 595.3X+2 224.2	0.998	0.025	7.0	67.4
47	倍氯米松	4.81	0.5~400	Y=820.6X+340.2	0.996	0.025	6.1	90.3
48	氟米松	4.62	0.5~400	Y=282.5X+86.0	0.996	0.025	6.7	84.1
49	地索奈德	4.98	0.5~400	Y=925.1X+114.0	0.999	0.025	3.0	99.6
50	甲基泼尼松龙醋酸酯	4.98	0.5~400	Y=1 975.0X+501.4	0.998	0.025	4.3	93.8
51	醋酸氟米龙	6.27	0.5~400	Y=1 558.0X+418.8	0.998	0.025	3.0	89.1
52	醋酸氟氢可的松	5.32	0.5~400	Y=68.6X-30.5	0.996	0.025	15.5	85.4
53	克林霉素	2.87	0.5~400	Y=4 334.8X+625.69	0.999	0.025	2.5	87.5
54	己酸羟孕酮	9.92	0.5~400	Y=907.5X+56.7	0.999	0.025	1.9	63.5
55	布地奈德	6.05	0.5~400	Y=993.4X+185.5	0.999	0.025	3.1	78.5
56	氢化可的松丁酸酯	6.13	0.5~400	Y=612.0X+126.0	0.996	0.025	3.4	86.3
57	醋酸倍他米松	6.02	0.5~400	Y=176.817X-16.8	0.998	0.025	6.3	72.1
58	氟尼缩松	4.96	0.5~400	Y=733.5X+135.8	0.998	0.025	3.9	89.7
59	地塞米松醋酸酯	5.84	0.5~400	Y=143.5X-3.9	0.998	0.025	5.7	91.1
60	曲安奈德	4.95	0.5~400	Y=568.9X+65.6	0.998	0.025	3.4	96.9
61	氟氢缩松	5.18	1.5~1 200	Y=35.2X-3.4	0.995	0.075	5.1	108.8
62	地夫可特	5.50	0.5~400	Y=1 194.6X+432.6	0.998	0.025	2.7	98.5
63	多西环素	2.77	0.5~400	Y=573.4X-126.0	0.999	0.025	17.9	100.2
64	卤米松	5.54	1.5~1 200	Y=142.5X+195.3	0.997	0.075	5.4	120.3
65	四环素	1.31	0.5~400	Y=353.8X-169.5	0.998	0.025	12.1	98.6
66	戊酸氢化可的松	6.76	0.5~400	Y=528.8X+97.5	0.998	0.025	3.2	82.2
67	氟轻松	5.13	0.5~400	Y=448.8X+95.3	0.996	0.025	3.5	100.8
68	哈西奈德	7.49	1.5~1 200	Y=96.0X+96.8	0.997	0.075	5.0	106.6
69	米诺环素	1.39	0.5~400	Y=863.4X-531.3	0.998	0.025	18.0	105.8
70	土霉素	1.10	0.5~400	Y=290.6X-198.8	0.995	0.025	16.4	99.5
71	氯倍他索丙酸酯	7.70	0.5~400	Y=703.2X+203.5	0.998	0.025	4.1	91.0
72	氯替泼诺	7.58	0.5~400	Y=1 916.9X+402.0	0.999	0.025	2.9	94.3
73	曲安奈德醋酸酯	6.72	0.5~400	Y=438.3X+72.7	0.997	0.025	4.2	88.5
74	倍他米松戊酸酯	7.22	0.5~400	Y=1 368.7X+198.7	0.999	0.025	4.2	97.1
75	金霉素	2.50	0.5~400	Y=95.7X-44.3	0.997	0.025	19.0	92.1
76	曲安西龙双醋酸酯	5.12	0.5~400	Y=865.7X+173.4	0.997	0.025	4.1	93.5
77	戊酸双氟可龙	8.51	0.5~400	Y=369.8X+63.1	0.997	0.025	4.8	65.0
78	丁酸氯倍他松	8.58	0.5~400	Y=353.2X-10.8	0.999	0.025	3.2	77.2
79	卤倍他索丙酸酯	7.64	0.5~400	Y=177.9X+17.5	0.995	0.025	6.8	101.5
80	泼尼卡酯	7.52	0.5~400	Y=2 350.4X+590.7	0.997	0.025	2.1	96.0
81	二氟拉松双醋酸酯	6.81	0.5~400	Y=696.7X+91.6	0.998	0.025	3.1	100.0
82	氟轻松醋酸酯	6.80	0.5~400	Y=813.3X+193.3	0.997	0.025	4.8	92.7
83	氟替卡松丙酸酯	7.80	0.5~400	Y=664.8X+111.0	0.997	0.025	3.7	100.5
84	安西奈德	7.64	0.5~400	Y=777.5X+211.7	0.996	0.025	1.9	98.0
85	倍他米松双丙酸酯	7.99	0.5~400	Y=1 315.0X+245.8	0.998	0.025	3.3	93.3
86	莫米他松糠酸酯	8.33	0.5~400	Y=1 714.7X+183.4	0.999	0.025	3.5	91.0
87	阿氯米松双丙酸酯	7.66	0.5~400	Y=586.3X+116.9	0.998	0.025	4.1	99.5
88	倍氯米松双丙酸酯	7.85	0.5~400	Y=895.6X+217.8	0.998	0.025	3.8	104.6
89	酮康唑	4.88	0.5~400	Y=790.0X+21.7	0.999	0.025	3.3	105.5
90	环索奈德	10.59	0.5~400	Y=3 332.5X+729.2	0.998	0.025	2.8	68.7
91	克拉霉素	5.18	0.5~400	Y=17 379.4X+2 710.0	0.999	0.025	2.9	100.9
92	阿奇霉素	5.18	0.5~400	Y=3 869.6X+435.1	0.999	0.025	4.4	101.1
93	罗红霉素	5.29	0.5~400	Y=9 042.4X+545.3	0.999	0.025	3.9	97.7
94	氯霉素	3.18	2.0~1 600	Y=4.3X+9.1	0.996	0.025	7.8	67.3

Tab. 2

References 13

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Simultaneous determination of 94 kinds of illegally added compounds in cosmetics by ultra performance liquid chromatography-tandem mass spectrometry

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