超高效液相色谱-串联质谱法测定化妆品中38种抗感染药

doi:10.3969/j.issn.1001-1803.2022.02.015

Abstract

Abstract:

An ultra high performance liquid chromatography-tandem mass spectrometric method was established for the determination of 38 forbidden anti-infective drugs in 2 matrixes of cosmetics. The cosmetic samples were extracted with solvent and performed on a Waters BEH C₁₈ （2.1 mm×100 mm, 1.7 μm） column with binary mobile phase consisting of 0.1% ammonium acetate pH=4.0 （solvent A） and 0.1% formic acid methanol solution （B） with gradient elution. Samples were analyzed by electronic spray ionization under a positive ion or negative ion mode with multiple reaction monitoring （MRM）, and then quantified by an external standard curve. The calibration curve of chloramphenicol is linear within the range of 100-1 000 μg/L and the calibration curves of the other 37 target compounds are linear within the range of 15-150 μg/L with the correlation coefficients above 0.99. The limits of detection （LOD） and limits of quantitation （LOQ） are in the ranges of 0.3-240.4 μg/kg and 1.1-801.2 μg/kg, respectively. The recoveries for 38 prohibited anti-infective drugs at three spiked levels are in the range of 79.0%-119.8% with the relative standard deviations （RSD） of 0.3%-9.7%（n=6）. The method is simple, rapid and accurate, and quite suitable for the simultaneous determination of illegally added anti-infective drugs in aqueous and cream cosmetics.

Key words: cosmetics, ultra high performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）, prohibited drugs, anti-infective drugs

CLC Number:

TQ658

Lu Linling,Qian Yefei,Zhang Bin,Lu Hui,Chen Libo,Min Chunyan,Chen Wei. Determination of 38 anti-infective drugs in cosmetics by ultra high performance liquid chromatography-tandem mass spectrometry[J].China Surfactant Detergent & Cosmetics, 2022, 52(2): 214-223.

Figures/Tables 5

Tab. 1

Fig.1

Tab. 2

Linear ranges, regression equations, coefficients of correlation, limits of detection and limits of quantitation of 38 forbidden anti-infective drugs in aqueous and cream cosmetics"

物质名称	基质类型	线性方程	相关系数r	线性范围/（ng/mL）	LOD/（μg/kg）	LOQ/（μg/kg）
甲硝唑	水剂	Y=3.90×10²X+7.01×10²	0.998 2	17.14~171.41	26.6	88.6
甲硝唑	膏霜	Y=3.29×10²X-1.75×10²	0.997 8	17.14~171.41	71.4	238.1
磺胺吡啶	水剂	Y=4.06×10³X-4.55×10³	0.999 6	15.16~151.62	18.4	61.5
磺胺吡啶	膏霜	Y=3.80×10³X-1.55×10⁴	0.997 4	15.16~151.62	52.5	174.9
磺胺甲嘧啶	水剂	Y=3.88×10³X-4.27×10³	0.999 3	16.04~160.44	11.3	37.6
磺胺甲嘧啶	膏霜	Y=4.00×10³X-1.10×10⁴	0.997 3	16.04~160.44	8.3	27.7
磺胺甲二唑	水剂	Y=3.17×10³X-2.25×10¹	0.998 7	17.44~174.43	5.6	18.8
磺胺甲二唑	膏霜	Y=3.26×10³X-6.90×10³	0.997 1	17.44~174.43	16	53.4
磺胺甲氧嗪	水剂	Y=4.95×10³X+1.53×10³	0.998 3	16.77~167.66	6.8	22.7
磺胺甲氧嗪	膏霜	Y=5.23×10³X-5.82×10³	0.998 8	16.77~167.66	24.3	81.1
磺胺氯哒嗪	水剂	Y=2.92×10³X-4.18×10³	0.999 6	15.61~156.05	13.8	45.9
磺胺氯哒嗪	膏霜	Y=3.08×10³X-5.63×10³	0.998 7	15.61~156.05	13.2	44.2
诺氟沙星	水剂	Y=4.50×10³X-3.60×10²	0.998 9	17.14~171.39	8.2	27.4
诺氟沙星	膏霜	Y=4.93×10³X-1.24×10⁴	0.999 1	17.14~171.39	5.7	19
依诺沙星	水剂	Y=7.41×10³X+1.25×10⁴	0.998 8	17.58~175.82	3.1	10.4
依诺沙星	膏霜	Y=8.29×10³X-2.33×10⁴	0.998 8	17.58~175.82	4.9	16.3
呋喃它酮	水剂	Y=3.09×10³X-2.98×10³	0.997 9	17.46~174.64	0.7	2.3
呋喃它酮	膏霜	Y=3.28×10³X-3.54×10³	0.997 8	17.46~174.64	0.7	2.3
培氟沙星	水剂	Y=1.45×10⁴X-2.79×10³	0.998 8	16.29~162.90	2.5	8.4
培氟沙星	膏霜	Y=1.65×10⁴X-2.73×10⁴	0.998 9	16.29~162.90	5.2	17.2
氧氟沙星	水剂	Y=2.54×10⁴X+5.33×10⁴	0.998 6	17.37~173.75	1.5	4.9
氧氟沙星	膏霜	Y=2.83×10⁴X-7.35×10²	0.998 6	17.37~173.75	2.8	9.2
氟罗沙星	水剂	Y=2.14×10⁴X+9.70×10³	0.999 1	16.41~164.05	0.8	2.8
氟罗沙星	膏霜	Y=2.27×10⁴X+3.05×10³	0.999 1	16.41~164.05	1.4	4.8
林可霉素	水剂	Y=4.64×10³X-2.63×10³	0.991 3	16.72~167.19	5.3	17.8
林可霉素	膏霜	Y=4.57×10³X-2.60×10⁴	0.995 8	16.72~167.19	1.9	6.5
磺胺甲恶唑	水剂	Y=2.18×10³X+1.50×10³	0.998 8	16.72~167.16	35.8	119.4
磺胺甲恶唑	膏霜	Y=2.14×10³X-1.64×10³	0.999 0	16.72~167.16	107.5	358.2
氟康唑	水剂	Y=3.69×10³X-5.91×10³	0.999 5	16.74~167.36	2.6	8.5
氟康唑	膏霜	Y=3.95×10³X-1.35×10²	0.998 2	16.74~167.36	3.8	12.6
环丙沙星	水剂	Y=8.35×10³X-3.23×10³	0.998 6	16.44~164.41	5.9	19.7
环丙沙星	膏霜	Y=9.31×10³X-1.38×10⁴	0.998 8	16.44~164.41	8.3	27.7
恩诺沙星	水剂	Y=1.54×10⁴X-5.16×10³	0.998 9	17.49~174.93	2.5	8.2
恩诺沙星	膏霜	Y=1.73×10⁴X+1.08×10⁴	0.999 6	17.49~174.93	2.3	7.5
沙拉沙星	水剂	Y=8.61×10³X+4.61×10³	0.996 5	15.52~155.25	2.5	8.3
沙拉沙星	膏霜	Y=9.32×10³X+2.50×10³	0.999 1	15.52~155.25	0.9	3.0
双氟沙星	水剂	Y=1.28×10⁴X-6.03×10³	0.998 5	16.49~164.88	2.3	7.6
双氟沙星	膏霜	Y=1.47×10⁴X-8.97×10³	0.998 8	16.49~164.88	2.9	9.6
莫西沙星	水剂	Y=7.72×10³X-3.15×10³	0.998 0	12.30~122.99	4.9	16.2
莫西沙星	膏霜	Y=8.32×10³X+1.30×10³	0.999 3	12.30~122.99	5.4	17.9
克林霉素	水剂	Y=3.22×10³X-4.37×10³	0.999 7	13.13~131.32	6.5	21.6
克林霉素	膏霜	Y=3.12×10³X+9.74×10²	0.999 5	13.13~131.32	1.9	6.2
四环素	水剂	Y=9.19×10²X-2.88×10³	0.994 8	16.24~162.38	53.1	176.9
四环素	膏霜	Y=1.02×10³X-3.32×10³	0.998 5	16.24~162.38	62.8	209.2
多西环素	水剂	Y=4.31×10³X-1.21×10⁴	0.997 2	17.19~171.89	17.5	58.2
多西环素	膏霜	Y=5.160×10³X-2.59×10⁴	0.997 1	17.19~171.89	24.2	80.5
米诺环素	水剂	Y=1.96×10³X-7.66×10³	0.994 0	16.97~169.65	51.8	172.8
米诺环素	膏霜	Y=2.00×10³X-9.58×10³	0.998 8	16.97~169.65	55.8	186
土霉素	水剂	Y=5.04×10²X-1.25×10³	0.998 7	16.40~164.00	81.7	272.4
土霉素	膏霜	Y=5.39×10²X+5.46×10¹	0.999 5	16.40~164.00	64.6	215.2
金霉素	水剂	Y=5.65×10²X-1.98×10³	0.992 4	16.02~160.25	68.1	226.9
金霉素	膏霜	Y=6.53×10²X-2.95×10³	0.999 1	16.02~160.25	148.3	494.5
克林霉素磷酸酯	水剂	Y=1.09×10³X-5.95×10³	0.991 4	14.25~142.51	3.5	11.6
克林霉素磷酸酯	膏霜	Y=1.16×10³X-5.34×10³	0.997 0	14.25~142.51	3.6	11.9
阿奇霉素	水剂	Y=1.23×10³X+1.32×10³	0.993 1	16.72~167.18	0.5	1.8
阿奇霉素	膏霜	Y=1.24×10³X-2.73×10³	0.998 7	16.72~167.18	0.5	1.8
克霉唑	水剂	Y=1.22×10⁴X-6.00×10³	0.999 3	16.99~169.88	0.7	2.3
克霉唑	膏霜	Y=1.43×10⁴X-4.74×10⁴	0.999 4	16.99~169.88	0.8	2.8
萘替芬	水剂	Y=3.28×10⁴X-8.62×10³	0.999 4	16.96~169.57	0.4	1.2
萘替芬	膏霜	Y=3.22×10⁴X+4.71×10⁴	0.998 5	16.96~169.57	0.4	1.2
螺内酯	水剂	Y=2.57×10³X+5.23×10²	0.997 1	16.53~165.25	2.4	8.2
螺内酯	膏霜	Y=2.57×10³X-6.23×10	0.998 5	16.53~165.25	3.4	11.4
灰黄霉素	水剂	Y=1.28×10⁴X-4.14×10²	0.998 3	16.49~164.92	0.7	2.5
灰黄霉素	膏霜	Y=1.34×10⁴X-1.32×10⁴	0.999 6	16.49~164.92	1.0	3.3
咪康唑	水剂	Y=4.13×10⁴X+2.35×10⁴	0.998 6	16.79~165.95	0.5	1.6
咪康唑	膏霜	Y=4.19×10⁴X+9.26×10⁴	0.997 7	16.79~165.95	0.5	1.5
酮康唑	水剂	Y=5.45×10³X-1.57×10⁴	0.993 9	15.64~156.41	0.8	2.7
酮康唑	膏霜	Y=5.08×10³X+4.21×10³	0.996 2	15.64~156.41	1.3	4.3
克拉霉素	水剂	Y=1.20×10³X-7.10×10²	0.995 0	22.76~227.55	16.0	53.3
克拉霉素	膏霜	Y=1.43×10³X-7.86×10³	0.996 6	22.76~227.55	16.0	53.3
罗红霉素	水剂	Y=9.1×10³X-8.73×10¹	0.996 8	15.24~152.42	0.3	1.1
罗红霉素	膏霜	Y=8.95×10³X+4.30×10¹	0.998 2	15.24~152.42	0.3	1.1
联苯苄唑	水剂	Y=9.49×10³X+4.02×10³	0.998 5	16.59~165.95	1.7	5.8
联苯苄唑	膏霜	Y=1.01×10⁴X-8.76×10³	0.999 6	16.59~165.95	1.2	3.9
氯霉素	水剂	Y=3.86×10¹X+1.75×10³	0.994 0	100.95~1 009.48	240.4	801.2
氯霉素	膏霜	Y=4.04×10¹X+8.71×10²	0.997 6	100.95~1 009.48	237.3	791.1

Tab. 2

Tab. 3

Results of recovery test and RSD （n=3） of 38 anti-infective drugs"

编号	物质名称	基质	平均回收率/%	RSD/%
1	甲硝唑	水液类	92.6,86.1,101.0	8.5,6.0,7.4
1	甲硝唑	霜乳类	89.4,81.7,97.3	8.0,1.4,5.8
2	磺胺吡啶	水液类	80.3,93.2,93.9	8.0,6.4,1.6
2	磺胺吡啶	霜乳类	114.9,113.2,93.4	7.3,3.6,2.3
3	磺胺甲嘧啶	水液类	105.7,94.4,94.1	8.9,3.8,0.4
3	磺胺甲嘧啶	霜乳类	119.6,96.5,95.0	9.7,8.3,7.9
4	磺胺甲二唑	水液类	97.3,91.6,97.1	3.5,3.1,2.1
4	磺胺甲二唑	霜乳类	113.2,104.0,99.8	9.5,3.0,2.5
5	磺胺甲氧嗪	水液类	99.9,96.2,98.0	4.8,0.5,0.3
5	磺胺甲氧嗪	霜乳类	108.1,84.9,85.5	6.8,6.7,5.5
6	磺胺氯哒嗪	水液类	93.0,99.0,95.9	4.5,7.9,1.3
6	磺胺氯哒嗪	霜乳类	90.8,92.1,93.3	8.2,4.6,3.2
7	诺氟沙星	水液类	98.4,98.8,102.3	6.3,1.0,0.6
7	诺氟沙星	霜乳类	90.5,94.3,99.9	7.2,6.8,2.2
8	依诺沙星	水液类	105.6,99.7,99.9	3.0,2.9,2.2
8	依诺沙星	霜乳类	105.0,101.4,90.6	9.1,8.4,5.2
9	呋喃它酮	水液类	102.1,103.0,99.0	4.1,2.4,1.3
9	呋喃它酮	霜乳类	94.2,90.4,95.7	9.2,7.6,2.1
10	培氟沙星	水液类	100.0,100.0,99.7	1.6,0.3,1.4
10	培氟沙星	霜乳类	99.1,93.0,95.6	1.3,4.5,2.2
11	氧氟沙星	水液类	107.3,100.1,100.3	3.3,0.8,1.2
11	氧氟沙星	霜乳类	106.0,96.3,96.8	4.3,4.9,1.4
12	氟罗沙星	水液类	115.7,101.7,101.9	5.6,1.1,0.7
12	氟罗沙星	霜乳类	99.4,92.5,91.0	6.0,1.7,9.2
13	林可霉素	水液类	90.2,103.8,101.3	9.5,1.1,2.5
13	林可霉素	霜乳类	100.0,91.5,100.3	4.3,5.0,3.5
14	磺胺甲噁唑	水液类	88.3,91.3,92.1	9.6,3.4,5.0
14	磺胺甲噁唑	霜乳类	111.9,92.6,90.3	8.1,6.8,4.0
15	氟康唑	水液类	111.4,103.0,100.3	7.9,1.8,1.9
15	氟康唑	霜乳类	102.7,82.9,97.7	1.9,9.0,3.0
16	环丙沙星	水液类	101.7,100.3,100.8	1.0,0.6,1.8
16	环丙沙星	霜乳类	97.5,95.5,99.5	4.6,4.6,2.5
17	恩诺沙星	水液类	105.2,100.8,100.8	1.4,1.0,1.5
17	恩诺沙星	霜乳类	98.6,92.9,103.2	3.1,4.2,0.6
18	沙拉沙星	水液类	103.8,104.6,101.2	3.2,6.9,0.9
18	沙拉沙星	霜乳类	93.4,95.5,100.2	8.2,3.9,4.6
19	双氟沙星	水液类	105.3,103.5,103.6	2.8,2.5,2.9
19	双氟沙星	霜乳类	99.8,95.1,103.2	1.6,2.9,3.0
20	莫西沙星	水液类	101.8,99.8,96.7	3.7,3.4,1.1
20	莫西沙星	霜乳类	101.5,94.1,105.1	2.2,5.2,3.5
21	克林霉素	水液类	97.2,99.8,98.1	4.8,1.6,0.6
21	克林霉素	霜乳类	93.4,93.1,97.7	4.4,3.7,3.7
22	四环素	水液类	108.5,101.7,98.4	8.6,4.3,7.4
22	四环素	霜乳类	108.5,95.3,99.1	1.0,10.5,3.5
23	多西环素	水液类	102.5,84.4,99.0	8.9,1.5,2.1
23	多西环素	霜乳类	108.9,91.4,114.3	7.2,7.5,8.3
24	米诺环素	水液类	79.5,87.6,100.2	9.8,8.5,6.8
24	米诺环素	霜乳类	113.4,85.8,105.9	5.2,9.8,6.0
25	土霉素	水液类	88.7,103.1,96.7	8.3,4.4,0.4
25	土霉素	霜乳类	85.4,100.5,98.7	6.9,8.4,6.9
26	金霉素	水液类	106.5,83.4,103.2	1.8,7.7,9.3
26	金霉素	霜乳类	106.9,91.5,90.7	3.6,8.9,5.7
27	克林霉素磷酸酯	水液类	93.7,95.5,96.4	5.6,9.9,3.7
27	克林霉素磷酸酯	霜乳类	80.1,100.3,106.2	5.6,4.3,6.3
28	阿奇霉素	水液类	103.7,92.7,104.6	2.9,4.6,3.4
28	阿奇霉素	霜乳类	118.4,112.1,102.8	7.3,7.2,3.2
29	克霉唑	水液类	91.7,97.2,96.3	4.0,3.1,4.9
29	克霉唑	霜乳类	91.3,85.6,97.2	8.2,5.7,0.6
30	萘替芬	水液类	97.9,99.5,96.6	4.8,3.9,2.3
30	萘替芬	霜乳类	83.5,79.0,94.5	5.4,7.0,2.9
31	螺内酯	水液类	97.9,98.8,96.9	3.1,4.6,4.0
31	螺内酯	霜乳类	86.2,80.1,90.4	8.3,9.7,3.7
32	灰黄霉素	水液类	90.1,101.9,89.8	5.4,3.7,8.9
32	灰黄霉素	霜乳类	89.7,93.7,100.8	9.6,3.6,1.1
33	咪康唑	水液类	102.2,100.5,100.7	2.9,2.3,1.2
33	咪康唑	霜乳类	96.4,96.9,89.4	0.7,2.6,5.1
34	酮康唑	水液类	107.0,98.9,98.4	4.5,1.5,1.3
34	酮康唑	霜乳类	98.7,99.6,102.1	1.1,2.1,3.7
35	克拉霉素	水液类	117.9,119.8,106.6	6.7,3.8,7.4
35	克拉霉素	霜乳类	95.7,87.7,90.1	3.2,0.8,5.6
36	罗红霉素	水液类	99.7,105.9,96.8	4.9,2.4,4.3
36	罗红霉素	霜乳类	103.5,101.5,103.6	5.6,3.5,1.9
37	联苯苄唑	水液类	91.3,95.1,93.8	9.2,7.9,5.3
37	联苯苄唑	霜乳类	90.5,89.6,97.2	9.3,6.9,2.5
38	氯霉素	水液类	81.1,95.6,101.8	3.2,2.4,5.6
38	氯霉素	霜乳类	111.4,111.0,104.1	9.0,3.9,7.0

Tab. 3

Tab. 4

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编号	物质名称	母离子（m/z）	锥孔电压/V	子离子（m/z）	碰撞电压/V
1	甲硝唑	172.0	25	128.0^*/80.2	15/25
2	磺胺吡啶	250.0	10	156.0^*/92.0	16/26
3	磺胺甲嘧啶	265.0	22	155.9^*/171.9	18/15
4	磺胺甲二唑	271.1	30	156.0^*/92.0	15/25
5	磺胺甲氧嗪	281.1	35	92.0^*/156.0	25/25
6	磺胺氯哒嗪	285.0	20	155.9^*/92.0	15/28
7	诺氟沙星	320.2	40	276.2^*/233.0	18/23
8	依诺沙星	321.2	40	232.0^*/303.2	35/20
9	呋喃它酮	325.0	28	251.9^*/281.0	15/12
10	培氟沙星	334.2	24	316.2^*/290.2	20/18
11	氧氟沙星	362.2	2	318.2^*/261.1	18/26
12	氟罗沙星	370.2	30	326.2^*/269.1	18/24
13	林可霉素	407.4	40	126.2^*/359.4	25/20
14	磺胺甲噁唑	254.0	22	155.8^*/107.9	18/18
15	氟康唑	307.0	2	220.0^*/238.0	16/15
16	环丙沙星	332.2	36	314.2^*/288.2	22/16
17	恩诺沙星	360.2	14	342.2^*/316.2	20/18
18	沙拉沙星	386.2	40	342.2^*/299.1	18/28
19	双氟沙星	400.2	54	382.2^*/356.2	16/18
20	莫西沙星	402.2	42	384.2^*/364.2	22/22
21	克林霉素	425.2	20	377.2^*/125.9	18/25
22	四环素	445.3	38	410.1^*/427.3	18/12
23	多西环素	445.2	42	428.2^*/154.0	18/28
24	米诺环素	458.3	54	441.2^*/352.2	18/30
25	土霉素	461.2	20	426.2^*/443.3	16/12
26	金霉素	479.2	36	444.1^*/462.1	18/16
27	克林霉素磷酸酯	505.2	68	126.1^*/457.2	28/20
28	阿奇霉素	749.9	55	591.6^*/115.7	30/40
29	克霉唑	277.0	4	241.0^*/165.0	20/24
30	萘替芬	288.0	20	117.0^*/141.0	25/15
31	螺内酯	341.2	56	107.0^*/187.1	28/20
32	灰黄霉素	353.0	40	215.0^*/165.0	20/20
33	咪康唑	417.0	60	161.0^*/159.0	30/28
34	酮康唑	531.3	26	489.3^*/255.0	28/30
35	克拉霉素	749.0	35	157.8^*/590.6	30/20
36	罗红霉素	837.5	22	158.2^*/679.4	31/36
37	联苯苄唑	311.0	20	243.0^*/165.0	15/10
38	氯霉素	321.2	25	152.2^*/257.2	15/10

编号	样品名称	批号	检出成分	含量/（mg/g）
1	妍菲妮嫩肤清滢祛痘霜	不详	甲硝唑	9.03
2	韩圣医紫草祛痘精油	不详	环丙沙星	7.75
3	神农本草精华霜	不详	氧氟沙星	3.08
3	神农本草精华霜	不详	甲硝唑	10.12
4	祛痘精华液	16032001	未检出	—
5	协和祛痘凝胶	160627	未检出	—
6	祛痘凝露	20160120	未检出	—
7	韩束祛痘舒缓精华水	F6031002	未检出	—
8	韩束茶树精油祛痘面膜	20210110A5TBUS	未检出	—
9	皮特灵系列祛痘护肤粉（浓缩）	不详	未检出	—
10	吾尊动能多效控油祛痘洁面膏	G5040902	未检出	—

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Determination of 38 anti-infective drugs in cosmetics by ultra high performance liquid chromatography-tandem mass spectrometry

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