基于UPLC-Q-TOF-MS与HPLC-QQQ-MS/MS对化妆品中23种局部麻醉药进行筛查与测定

doi:10.3969/j.issn.2097-2806.2026.02.015

Abstract

Abstract:

The laboratory established an efficient reversed-phase ultra-high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry（UPLC-Q-TOF-MS）qualitative method for screening more than 2 000 kinds of risk substances（including local anesthetics, LAs）in cosmetics, which has been successfully applied in the analysis of actual samples. This work aims to develop a more convenient high performance liquid chromatography triple quadrupole mass spectrometry（HPLC-QQQ-MS/MS）method for the quantitative determination of LAs. Samples were ultrasonically extracted with methanol, separated on an Agilent Poroshell 120 EC-C₁₈ column（2.1 mm × 100 mm, 2.7 μm）, and eluted with a gradient mobile phase consisting of 0.1% formic acid aqueous solution and methanol. Quantification was performed using the external standard method. The results show that all 23 LAs are effectively separated within 12 minutes, with good linearity in the corresponding concentration ranges and the correlation coefficients all greater than 0.99. The limits of detection（LOD）range from 0.002 5 to 0.05 μg/g, and the limits of quantification（LOQ）range from 0.01 to 0.1 μg/g. The average recoveries of the 23 LAs in 5 blank cosmetic matrices are 80.68%-117.57%, with the relative standard deviations（RSDs）less than 5.98%. This method has good precision and high accuracy, and is suitable for the determination of LAs in 5 cosmetic matrices.

Key words: local anesthetics, chemical analysis, ultra-high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry（UPLC-Q-TOF-MS）, high performance liquid chromatography triple quadrupole mass spectrometry（HPLC-QQQ-MS/MS）

CLC Number:

TQ658

Ruotong Yang, Fangyuan Wu, Guangqian Xu, Guiwen Guo, Haiyan Wang, Lingyun Jia. Screening and determination of 23 local anesthetics in cosmetics using UPLC-Q-TOF-MS and HPLC-QQQ-MS/MS[J].China Surfactant Detergent & Cosmetics, 2026, 56(2): 260-270.

Figures/Tables 9

Tab.1

Fig.1

Fig.2

Fig.3

Tab.2

Linear equations and correlation coefficients of 23 LAs"

No.	Lotion		Cream		Gel		Oil		Powder		LOD/ （μg/g）	LOQ/ （μg/g）
No.	Linear equation	r	Linear equation	r	Linear equation	r	Linear equation	r	Linear equation	r	LOD/ （μg/g）	LOQ/ （μg/g）
1	y=2 769x+313	0.995 9	y=20 514x+222	0.998 1	y=20 332x+353	0.9971	y=11 906x-24 142	0.997 0	y=16 005x+834	0.993 8	0.01	0.025
2	y=3 596x-651	0.992 2	y=21 525x+1 357	0.996 3	y=21 504x+306	0.9992	y=24 247x+9 634	0.997 9	y=15 804x+1 225	0.993 9	0.006	0.02
3	y=7 203x+107	0.999 6	y=7 911x-546	0.999 5	y=8 309x-3 537	0.9999	y=17 451x-10 680	0.997 3	y=14 822x-5 011	0.998 1	0.025	0.1
4	y=132 147x-998	0.999 2	y=122 344x+2 480	0.995 3	y=140 572x+2 552	0.9985	y=278 206x+39 388	0.993 0	y=126 860x+2 475	0.995 9	0.002 5	0.005
5	y=181 138x-83	0.998 8	y=182 089x+649	0.999 2	y=182 374x+2 203	0.9971	y=232 382x+151 973	0.993 4	y=121 044x+2 878	0.994 0	0.002 5	0.005
6	y=1 098x-21	0.994 9	y=1 090x-321	0.998 9	y=1 023x+1 931	0.9980	y=6 132x+4 465	0.997 5	y=1 005x+1 089	0.991 4	0.05	0.1
7	y=19 024x+687	0.994 8	y=18 581x-1 419	0.996 6	y=20 058x-16	0.9950	y=18 801x+17 176	0.997 8	y=4 889x+5 615	0.993 7	0.005	0.025
8	y=17 328x+144	0.997 0	y=14 511x-187	0.998 9	y=17 547x+721	0.9992	y=20 757x-16 492	0.993 2	y=19 127x+731	0.992 0	0.005	0.025
9	y=162 451x+3 558	0.997 5	y=120 894x+795	0.999 4	y=161 256x+8 905	0.9957	y=176 537x+158 195	0.992 9	y=77 893x+16 549	0.990 1	0.005	0.025
10	y=88 897x+17 572	0.997 9	y=61 738x+7 070	0.994 3	y=89 474x+36 148	0.9949	y=102 930x+56 070	0.993 7	y=69 698x+10 303	0.992 8	0.005	0.025
11	y=39 477x+506	0.998 6	y=40 530x+592	0.995 9	y=36 668x+1 225	0.9973	y=1 435x-1 937	0.993 9	y=44 163x-1 183	0.997 6	0.01	0.03
12	y=6 401x-397	0.997 6	y=7 217x+94	0.999 0	y=6 907x-460	0.9972	y=63 891x+464	0.991 4	y=7 082x+441	0.997 4	0.02	0.05
13	y=716x+229	0.997 3	y=725x+2 255	0.995 7	y=651x+536	0.9926	y=1 040x+419	0.993 6	y=158 812x+3 719	0.990 6	0.025	0.05
14	y=72 613x+3 039	0.994 2	y=64 075x+796	0.998 5	y=61 454x+1 438	0.9933	y=86 627x+71 404	0.998 6	y=157 162x+4 057	0.990 4	0.002 5	0.01
15	y=36 323x+3 125	0.999 2	y=33 109x-3 211	0.999 1	y=36 910x+4 529	0.9990	y=45 302x+27 275	0.997 5	y=27 520x+609	0.994 3	0.005	0.025
16	y=29 030x+3 013	0.997 1	y=20 748x+6 754	0.995 9	y=21 832x+5 406	0.9916	y=41 723x+13 281	0.990 8	y=24 930x+1 377	0.991 3	0.005	0.02
17	y=271 458x+5 093	0.994 7	y=227 299x+21 757	0.999 2	y=246 299x+11 845	0.9930	y=192 135x+14 084	0.992 1	y=150 443x+12 488	0.990 0	0.005	0.025
18	y=30 188x+67	0.999 4	y=31 528x+5 638	0.997 9	y=31 870x+3 460	0.9994	y=31 920x+12 809	0.998 9	y=24 352x+647	0.998 9	0.01	0.03
19	y=40 949x+5 432	0.991 1	y=47 461x+4 512	0.998 0	y=43 106x+5 827	0.9956	y=20 473x+2 847	0.995 0	y=30 531x+1 459	0.994 2	0.005	0.025
20	y=26 281x+2 147	0.991 8	y=26 394x+443	0.997 1	y=19 371x+1 249	0.9944	y=30 791x+3 835	0.992 3	y=37 154x+764	0.993 9	0.004 5	0.015
21	y=17 880x+423	0.999 9	y=19 342x+3 624	0.999 2	y=18 840x+3 204	0.9994	y=174 414x-11 574	0.999 1	y=9 637x+3 698	0.999 7	0.01	0.025
22	y=84 334x+19 710	0.999 5	y=149 989x+2 055	0.998 8	y=147 658x+5 085	0.9971	y=128 251x+1 701	0.992 1	y=106 380x+3 856	0.991 9	0.01	0.05
23	y=40 330x-8 018	0.998 1	y=95 197x+1 258	0.998 6	y=95 204x+1 323	0.9984	y=116 870x+90 393	0.997 3	y=41 016x+1 440	0.992 2	0.01	0.05

Tab.2

Tab.3

Accuracy results of 23 LAs"

No.	Concentration	Lotion		Cream		Gel		Oil		Power
No.	Concentration	Recovery/%	RSD/%	Recovery/%	RSD/%	Recovery/%	RSD/%	Recovery/%	RSD/%	Recovery/%	RSD/%
1	Low	89.69	2.61	89.63	4.13	84.31	1.61	107.27	3.16	110.36	1.34
1	High	83.34	2.48	94.93	1.41	84.97	2.05	107.27	1.10	92.96	0.83
2	Low	89.88	3.57	95.57	2.51	85.11	1.73	108.06	3.42	100.14	1.96
2	High	98.17	0.79	99.97	1.13	91.81	1.74	97.61	1.29	84.93	1.15
3	Low	87.67	1.13	89.66	1.68	95.95	1.42	105.68	0.99	81.41	1.77
3	High	90.04	2.65	96.06	1.47	98.97	2.38	108.32	4.24	90.20	1.82
4	Low	99.04	2.06	113.01	3.63	88.91	3.41	95.79	2.88	90.73	0.70
4	High	89.56	2.36	89.80	0.92	88.58	4.06	100.20	2.85	83.89	0.68
5	Low	92.98	1.08	93.76	0.43	86.42	2.05	99.47	2.34	83.99	0.78
5	High	90.45	2.23	90.23	1.78	101.07	2.33	92.27	2.44	103.67	1.90
6	Low	95.36	3.49	94.83	3.00	96.48	0.83	100.37	3.00	90.06	1.87
6	High	98.23	2.01	92.96	1.26	91.31	2.13	102.27	1.35	90.98	1.01
7	Low	87.54	2.42	99.73	2.24	90.17	4.03	97.18	4.00	105.24	1.33
7	High	89.76	2.44	107.01	2.17	89.65	1.60	104.41	1.76	91.05	1.70
8	Low	87.18	3.80	106.05	1.80	87.75	2.48	105.31	2.36	90.53	2.13
8	High	87.58	3.95	102.04	1.63	87.45	1.67	110.68	1.10	95.39	2.00
9	Low	100.25	2.35	115.39	2.72	89.37	2.92	106.65	3.51	95.76	1.16
9	High	89.77	2.25	102.01	1.13	86.54	1.69	112.99	2.12	109.97	1.74
10	Low	97.05	3.62	113.85	0.38	82.46	1.87	107.17	3.24	102.87	1.80
10	High	97.04	1.52	99.46	1.02	86.16	1.10	112.53	0.96	86.11	0.21
11	Low	92.68	3.21	105.56	3.49	86.13	4.07	113.18	0.36	87.93	2.97
11	High	91.30	1.32	87.88	3.90	90.53	2.96	107.94	3.27	98.06	2.78
12	Low	94.17	3.87	100.62	1.88	90.76	1.21	109.58	4.62	86.51	4.44
12	High	89.34	1.64	86.07	3.83	86.74	2.25	104.61	2.56	82.69	4.12
13	Low	97.44	3.37	92.62	2.84	100.36	1.53	112.47	2.98	116.10	2.70
13	High	95.69	3.66	85.28	2.88	97.25	2.06	112.70	2.66	98.83	1.30
14	Low	101.81	2.06	105.25	1.96	89.59	2.91	104.55	1.74	95.74	3.26
14	High	82.74	1.47	89.27	0.73	102.89	1.32	111.90	1.53	93.72	1.90
15	Low	91.13	3.87	103.37	1.64	96.67	1.48	113.13	2.42	82.07	4.73
15	High	88.66	1.32	100.31	2.26	95.97	1.31	108.60	2.45	80.45	0.63
16	Low	101.23	1.18	114.26	3.60	94.68	3.81	105.51	3.38	88.59	0.86
16	High	88.10	2.71	91.35	0.71	93.82	1.14	108.89	1.24	105.40	1.12
17	Low	94.19	0.92	97.03	1.89	91.73	1.49	107.76	1.43	109.32	4.94
17	High	93.12	1.32	85.71	1.93	98.77	1.76	101.60	2.12	100.58	0.85
18	Low	90.34	0.97	91.85	4.25	91.61	3.53	100.45	2.12	91.53	3.03
18	High	91.65	1.20	95.91	2.18	87.49	2.73	99.42	1.68	89.32	2.41
19	Low	101.53	1.23	112.23	4.71	102.31	2.58	110.64	2.26	107.54	3.37
19	High	89.92	2.72	99.86	2.52	99.40	3.01	110.21	2.54	95.07	2.53
20	Low	97.20	3.34	100.56	3.63	92.99	3.17	103.58	3.25	90.70	4.15
20	High	90.16	2.67	88.33	3.40	109.56	2.77	109.66	3.41	112.15	2.57
21	Low	91.87	2.38	88.93	1.85	101.55	2.55	109.44	4.23	96.40	3.94
21	High	89.23	2.42	89.15	3.36	92.75	1.96	106.20	1.72	95.70	3.05
22	Low	103.85	1.19	91.91	2.68	90.41	1.84	108.34	1.85	84.16	4.21
22	High	107.39	2.47	84.65	3.47	90.93	2.08	109.27	2.50	83.45	2.28
23	Low	99.33	1.98	97.41	2.87	88.78	2.52	92.26	3.93	109.25	3.89
23	High	88.70	1.36	94.85	1.63	105.04	1.19	98.40	1.68	101.86	1.82

Tab.3

Tab.4

Precision results of 23 LAs"

No.	Concentration	Lotion		Cream		Gel		Oil		Powder
No.	Concentration	Recovery/%	RSD/%	Recovery/%	RSD/%	Recovery/%	RSD/%	Recovery/%	RSD/%	Recovery/%	RSD/%
1	Low	90.25	3.94	90.74	4.40	84.22	1.80	106.42	4.79	110.16	4.99
	Middle	85.71	4.73	93.25	3.36	84.20	1.76	106.31	3.79	92.54	4.98
	High	84.32	3.08	95.58	2.88	84.90	3.43	109.92	4.81	99.77	4.85
2	Low	89.07	3.48	94.39	4.54	91.76	4.89	97.85	1.70	84.74	3.23
	Middle	92.52	2.92	106.14	4.25	95.85	2.85	104.20	5.98	81.52	2.23
	High	97.90	2.01	100.55	2.67	99.38	2.84	108.47	3.39	89.93	3.03
3	Low	87.41	0.85	90.28	3.12	89.12	3.26	95.65	4.33	91.25	3.73
	Middle	86.71	2.85	90.61	2.49	88.09	1.23	100.82	3.22	83.70	2.28
	High	89.85	1.73	96.26	2.30	86.47	1.87	101.13	3.37	83.91	1.57
4	Low	98.81	2.48	112.06	3.67	100.93	3.87	93.33	2.68	104.21	2.12
	Middle	92.61	2.20	96.63	1.96	96.01	1.54	100.02	2.25	90.65	1.16
	High	90.44	2.18	90.74	1.01	92.26	0.98	101.58	3.30	91.11	0.87
5	Low	93.60	1.78	93.20	2.66	90.16	1.64	97.93	4.46	105.43	1.97
	Middle	86.54	2.70	92.97	1.87	90.24	2.83	106.03	4.57	91.24	0.87
	High	89.18	2.90	89.21	1.72	88.81	2.83	105.85	4.37	91.13	2.43
6	Low	94.89	2.69	95.29	2.95	87.78	2.76	110.48	4.05	95.54	3.75
	Middle	96.06	2.88	92.09	1.62	88.74	2.60	107.51	3.57	96.39	3.34
	High	97.22	2.81	93.89	2.01	86.39	1.91	113.64	3.86	110.48	4.05
7	Low	88.50	3.97	98.65	3.09	83.05	1.95	107.32	4.57	102.36	4.57
	Middle	84.33	4.69	101.14	1.77	85.83	2.51	113.54	2.80	86.31	3.80
	High	89.18	3.82	107.49	3.20	85.41	2.69	112.41	1.54	88.04	2.76
8	Low	88.80	2.39	104.83	3.12	91.10	4.06	109.32	4.15	97.83	1.40
	Middle	87.31	1.98	103.16	1.82	90.23	1.41	109.79	2.23	84.91	1.57
	High	88.64	2.29	101.93	2.64	86.91	1.87	106.17	3.60	82.03	2.18
9	Low	99.68	2.59	113.01	4.93	100.61	1.77	113.64	3.32	117.52	1.63
	Middle	87.86	1.87	111.04	1.04	96.33	2.35	113.13	1.21	99.63	1.83
	High	88.63	2.28	102.01	2.01	89.86	2.35	103.51	1.81	94.94	1.33
10	Low	98.91	3.15	114.39	0.88	103.31	3.09	109.85	3.61	94.49	2.41
	Middle	100.25	3.80	104.95	1.14	97.94	1.11	111.99	1.84	83.12	1.81
	High	96.67	1.77	99.46	1.96	95.72	1.60	108.20	2.72	80.68	0.69
11	Low	92.18	3.58	104.03	4.41	95.32	4.35	104.61	4.89	88.33	4.85
	Middle	88.99	3.47	93.77	4.72	94.10	4.25	108.52	3.22	105.15	2.66
	High	92.20	4.66	87.88	3.76	92.28	4.22	107.91	2.65	107.73	2.60
12	Low	95.46	2.83	100.87	3.41	99.79	2.67	103.19	3.96	100.75	4.19
	Middle	93.05	1.98	89.90	3.48	92.17	1.95	101.67	3.67	90.80	2.18
	High	90.56	3.38	85.04	3.95	88.20	2.08	99.18	3.50	89.57	2.68
13	Low	96.94	2.00	93.05	4.80	103.25	3.63	108.08	2.89	109.95	1.32
	Middle	92.71	4.22	90.96	4.73	97.43	4.76	109.73	4.04	96.05	1.72
	High	95.17	1.90	85.28	2.62	91.57	4.95	104.44	3.16	91.98	1.09
14	Low	100.74	3.58	103.97	4.56	110.32	2.04	109.42	1.50	112.92	2.42
	Middle	92.67	2.87	93.52	2.51	101.27	2.74	110.28	3.23	96.18	1.90
	High	82.57	1.23	90.07	1.35	92.80	1.69	107.33	1.54	94.71	1.29
15	Low	92.15	3.26	104.17	3.88	91.11	1.55	108.57	2.16	84.47	1.08
	Middle	89.40	3.89	101.64	4.78	90.93	2.02	107.67	1.79	82.69	1.06
	High	88.16	2.26	101.25	1.55	87.99	2.51	93.00	2.90	108.57	2.16
16	Low	99.99	2.74	112.79	3.57	105.87	4.02	98.25	4.21	102.64	2.39
	Middle	93.81	2.51	97.58	2.18	93.62	2.08	100.14	2.41	91.08	2.86
	High	89.31	1.65	91.50	1.49	85.43	1.97	97.64	2.31	87.04	1.59
17	Low	93.80	1.68	95.92	1.99	94.03	2.80	100.13	3.26	111.12	0.95
	Middle	92.29	3.26	89.83	2.22	89.67	3.11	102.55	1.90	93.11	1.95
	High	92.73	1.41	87.04	3.39	88.22	2.40	100.97	1.79	93.51	1.56
18	Low	90.70	3.08	90.14	1.90	86.73	3.20	100.13	2.93	103.30	3.39
	Middle	87.87	1.40	91.43	1.19	85.75	1.80	110.50	3.57	95.27	2.41
	High	92.36	2.01	95.91	1.76	83.42	2.26	117.57	1.28	87.93	2.35
19	Low	100.67	2.62	112.23	2.66	92.53	3.11	114.88	2.31	97.06	3.84
	Middle	93.76	2.19	105.37	3.20	88.99	2.38	115.60	2.54	87.38	3.42
	High	89.08	2.43	99.86	1.67	85.08	2.68	109.35	2.51	95.21	2.44
20	Low	95.62	1.57	105.27	1.60	99.94	2.09	98.15	5.43	92.24	0.97
	Middle	92.32	2.19	91.26	2.00	93.80	2.38	98.16	4.12	82.61	1.96
	High	89.28	1.46	88.02	2.54	88.55	2.31	95.52	4.30	86.96	2.69
21	Low	91.62	2.10	88.29	1.51	91.34	2.63	95.42	4.10	100.12	4.21
	Middle	88.49	1.32	86.67	2.05	91.15	1.31	102.08	2.93	89.14	3.50
	High	89.71	1.98	87.85	1.24	90.23	1.71	102.49	4.78	84.93	3.07
22	Low	104.74	1.09	92.23	1.27	87.08	4.12	95.13	1.64	105.80	1.73
	Middle	105.18	1.64	86.00	1.70	86.60	1.64	100.21	2.62	92.25	1.60
	High	108.36	1.36	85.35	2.18	86.82	4.50	101.30	2.29	95.38	1.13
23	Low	98.48	2.20	98.20	4.71	99.45	2.43	115.07	1.83	101.36	2.49
	Middle	92.04	3.17	97.55	1.59	97.30	2.67	115.97	2.57	89.46	2.43
	High	89.22	3.32	94.51	2.52	89.98	2.75	114.80	1.64	87.11	2.69

Tab.4

Fig.4

Tab.5

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No.	Compound name	Precursor ion（m/z）	R_t/min	Product ion（m/z）	DP/V	CE/V
1	Procaine	237.2	1.23	99.9^*	72	17
1	Procaine	237.2	1.23	119.8	23	41
2	Procainamide	236.2	1.81	162.1^*	91	34
2	Procainamide	236.2	1.81	119.9	65	62
3	Chloroprocaine	271.1	4.37	197.8^*	60	26
3	Chloroprocaine	271.1	4.37	153.2	84	50
4	Lidocaine	235.2	4.83	86.1^*	71	25
4	Lidocaine	235.2	4.83	58.0	38	27
5	Mepivacaine	247.1	4.93	98.1^*	71	23
5	Mepivacaine	247.1	4.93	70.1	84	63
6	Prilocaine	221.1	5.03	85.9^*	53	66
6	Prilocaine	221.1	5.03	135.8	20	28
7	Dezocine	246.2	5.75	146.9^*	63	28
7	Dezocine	246.2	5.75	229.0	66	15
8	Cocaine	304.1	6.11	181.8^*	77	43
8	Cocaine	304.1	6.11	82.0	71	47
9	Ropivacaine	275.3	6.11	126.1^*	91	30
9	Ropivacaine	275.3	6.11	84.0	93	62
10	Proxymetacaine	295.2	6.32	99.9^*	23	22
10	Proxymetacaine	295.2	6.32	135.9	107	35
11	Piperocaine	261.7	6.37	104.8^*	49	39
11	Piperocaine	261.7	6.37	162.9	43	29
12	Xylazole	204.6	6.52	188.6^*	88	39
12	Xylazole	204.6	6.52	104.7	97	32
13	Dyclonine	289.4	6.68	97.9^*	110	22
13	Dyclonine	289.4	6.68	140.0	75	27
14	Bupivacaine	289.2	6.68	98.1^*	81	51
14	Bupivacaine	289.2	6.68	140.2	87	27
15	Butacaine	307.2	6.78	177.9^*	107	27
15	Butacaine	307.2	6.78	119.8	129	61
16	Oxybuprocaine	309.2	6.78	235.9^*	64	26
16	Oxybuprocaine	309.2	6.78	191.8	109	26
17	Tetracaine	265.2	6.98	176.0^*	28	21
17	Tetracaine	265.2	6.98	71.9	60	41
18	Tricaine	165.8	6.98	137.9^*	62	20
18	Tricaine	165.8	6.98	93.9	66	29
19	Midazolam	326.1	6.98	291.0^*	125	39
19	Midazolam	326.1	6.98	249.1	88	50
20	Pramoxine	294.2	7.40	150.9^*	75	29
20	Pramoxine	294.2	7.40	99.7	134	50
21	Benzocaine	166.2	7.55	120.0^*	61	28
21	Benzocaine	166.2	7.55	94.0	59	23
22	Cinchocaine	344.0	7.60	270.9^*	91	34
22	Cinchocaine	344.0	7.60	215.1	108	45
23	Quinisocaine	273.4	7.91	72.0^*	62	27
23	Quinisocaine	273.4	7.91	227.9	26	24

Positive samples	Compound name	Detection value/（μg/g）				Average value/ （μg/g）	RSD/ %
Positive samples	Compound name	Screening Platform	Validating institution 1	Validating institution 2	Validating institution 3	Average value/ （μg/g）	RSD/ %
Sample 1	Dyclonine	2.512	2.666	2.586	2.623	2.563	4.28
Sample 1	Dyclonine	2.426	2.733	2.545	2.496	2.563	4.28
Sample 2	Lidocaine	2.647	2.580	2.560	2.421	2.537	4.74
Sample 2	Lidocaine	2.665	2.567	2.480	2.427	2.537	4.74

Screening and determination of 23 local anesthetics in cosmetics using UPLC-Q-TOF-MS and HPLC-QQQ-MS/MS

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