超高效液相色谱-串联质谱法同时测定化妆品中29种抗过敏药物

doi:10.3969/j.issn.2097-2806.2023.07.014

Abstract

Abstract:

The study aims to develop an ultra high performance liquid chromatography-tandem mass spectrometry method for the determination of 29 anti-allergy drugs in cosmetics. The samples were extracted by ultrasonic machine with acetonitrile, and the separation was executed on a column using the mobile phase consisting of 0.1% ammonium hydroxide （A） and 0.1% ammonium hydroxide methanol solution （B）. The analysis was performed using a positive electrospray ion source in multiple reaction monitoring （MRM） mode. The result show that the linear relationship of the 29 anti-allergy drugs in the linear range is good, and the correlation coefficient is greater than 0.997. The detection limits are between 0.4-12.9 ng/g, and the average recovery rate is in the range of 80.9%-115.9%, with RSD within 0.3%-14.8%. 2 Batches of positive samples are detected within 10 batches of the samples, cyproheptadine and cyproheptadine impurity 1 are found in 1 batch, and cimetidine is found in 1 batch. The established method is simple, selective, sensitive and accurate, and can be used for the determination of anti-allergy drugs in cosmetics.

Key words: UPLC-MS/MS, cosmetics, anti-allergy drugs

CLC Number:

TQ658

Zheng Jiaxin, Jia Changping, Zhang Shanshan. Determination of 29 anti-allergy drugs by UPLC-MS/MS in cosmetics[J].China Surfactant Detergent & Cosmetics, 2023, 53(7): 833-840.

Figures/Tables 4

Tab. 1

Standard product information of 29 components"

编号	物质名称	纯度/%	批号	来源
1	曲吡那敏	99.98	TC191206	Stanford chemicals公司
2	阿司咪唑	100	100301-199901	中国食品药品检定研究院
3	赛庚啶	92.2	100502-201802	中国食品药品检定研究院
4	氯丙嗪	99.7	100460-201302	中国食品药品检定研究院
5	特非那定	99.4	100292-201302	中国食品药品检定研究院
6	司他斯汀	99.5	100686-202002	中国食品药品检定研究院
7	西咪替丁	99.8	100158-201406	中国食品药品检定研究院
8	二氧丙嗪	99.8	100299-201803	中国食品药品检定研究院
9	氯苯那敏	99.7	100047-202008	中国食品药品检定研究院
10	羟嗪	98.6	100266-200201	中国食品药品检定研究院
11	奋乃静	99.9	100133-201403	中国食品药品检定研究院
12	氯苯沙明	98.9	E0025179	曼哈格
13	奥洛他定	99.6	101098-201001	中国食品药品检定研究院
14	多西拉敏	98	E0025312	曼哈格
15	苯海拉明	99.9	100066-200807	中国食品药品检定研究院
16	氯雷他定	100	100615-201404	中国食品药品检定研究院
17	依匹斯汀	100	100510-200601	中国食品药品检定研究院
18	非索非那定	99.8	100852-201202	中国食品药品检定研究院
19	美沙吡林	99.5	E0025313	曼哈格
20	赛克利嗪	96.6	D0016335	曼哈格
21	卢帕他定	99.5	101241-201101	中国食品药品检定研究院
22	氟奋乃静	99.5	100162-201604	中国食品药品检定研究院
23	西替利嗪	99.3	100660-201102	中国食品药品检定研究院
24	酮替芬	99.8	100230-201904	中国食品药品检定研究院
25	溴苯那敏	99.4	G155522	Dr.Ehrenstorfer GmbH公司
26	地氯雷他定	99.8	100919-201904	中国食品药品检定研究院
27	二苯拉林	100 μg/mL	D0016315	曼哈格
28	赛庚啶杂质1	100	101411-201601	中国食品药品检定研究院
29	异丙嗪	99.5	100422-201603	中国食品药品检定研究院

Tab. 1

Tab. 2

Tab. 3

Linear range, linear equation, correlation coefficient and detection limit of the 29 anti-allergy drugs"

编号	物质名称	线性范围/ （ng/mL）	保留时间/min	线性方程	相关系数r	检出限/（ng/g）	定量限/（ng/g）
1	曲吡那敏	0.24~9.64	2.58	Y=2.16×10⁶ X+3.13×10⁵	0.999 3	2.7	8.9
2	阿司咪唑	0.28~11.09	2.81	Y=5.21×10⁵ X+4.09×10⁴	0.999 8	5.3	17.6
3	赛庚啶	0.28~11.24	3.03	Y=2.94×10⁵ X+846	0.999 9	4.1	13.6
4	氯丙嗪	0.28~11.02	3.33	Y=7.77×10⁵ X+4.83×10⁴	0.999 9	1.6	5.3
5	特非那定	0.26~10.40	3.77	Y=9.74×10⁵ X-1.42×10⁴	0.999 5	2.9	9.5
6	司他斯汀	0.36~14.28	4.31	Y=1.03×10⁶ X+6.80×10⁴	0.999 8	0.4	1.3
7	西咪替丁	0.26~10.29	0.33	Y=2.17×10⁵ X+3.48×10³	0.999 6	12.5	41.7
8	二氧丙嗪	0.25~9.90	0.50	Y=1.35×10⁵ X-1.36×10³	0.999 9	9.6	32.1
9	氯苯那敏	0.28~11.13	2.56	Y=1.64×10⁶ X+4.21×10⁴	0.999 8	4.7	15.6
10	羟嗪	0.29~11.70	2.68	Y=8.97×10⁵ X+1.44×10⁵	0.999 4	1.1	3.7
11	奋乃静	0.24~9.44	2.88	Y=5.77×10⁵ X+1.01×10⁴	0.999 9	4.0	13.4
12	氯苯沙明	0.25~9.89	3.16	Y=5.48×10⁴ X+1.40×10⁴	0.997 4	9.4	31.3
13	奥洛他定	0.25~9.88	0.33	Y=1.18×10⁵ X+1.88×10³	0.999 9	6.8	22.7
14	多西拉敏	0.25~9.80	2.52	Y=1.02×10⁶ X-5.79×10⁴	0.999 8	2.5	8.2
15	苯海拉明	0.29~11.46	2.68	Y=8.87×10⁵ X+9.46×10⁴	0.999 6	2.3	7.7
16	氯雷他定	0.27~10.87	2.74	Y=7.76×10⁵ X+6.40×10⁴	0.999 9	2.6	8.6
17	依匹斯汀	0.33~13.13	2.93	Y=2.84×10⁵ X+4.55×10⁴	0.999 9	4.2	13.9
18	非索非那定	0.29~11.52	0.32	Y=1.68×10⁵ X+8.99×10³	0.999 9	6.5	21.6
19	美沙吡林	0.25~9.84	2.52	Y=1.76×10⁶ X+3.44×10³	0.999 9	4.9	16.2
20	赛克利嗪	0.27~10.88	2.66	Y=2.72×10⁵ X+1.01×10⁴	0.999 9	5.4	18.1
21	卢帕他定	0.25~10.04	2.74	Y=2.34×10⁵ X+1.64×10⁴	0.999 5	5.8	19.2
22	氟奋乃静	0.26~10.27	2.92	Y=2.65×10⁵ X+2.14×10⁴	0.999 8	6.1	20.5
23	西替利嗪	0.34~13.46	0.33	Y=2.37×10⁵ X+2.97×10⁴	0.999 7	5.8	19.2
24	酮替芬	0.29~11.54	2.59	Y=4.12×10⁴ X+2.97×10³	0.999 3	4.1	13.6
25	溴苯那敏	0.28~11.14	2.64	Y=7.83×10⁵ X-3.37×10⁴	0.999 9	3.0	10.0
26	地氯雷他定	0.25~10.13	2.66	Y=8.66×10⁵ X-8.60×10⁴	0.998 3	1.2	3.9
27	二苯拉林	0.25~10.00	2.72	Y=6.28×10⁵ X+6.69×10⁴	0.999 5	7.5	25.0
28	赛庚啶杂质1	0.22~8.70	2.75	Y=1.86×10⁵ X+2.38×10⁴	0.999 0	2.7	8.9
29	异丙嗪	0.27~10.79	2.84	Y =4.84×10⁵ X+2.99×10⁴	0.999 8	12.9	43.1

Tab. 3

Tab. 4

Precisions and recoveries （n=6）"

编号	物质名称	添加水平/（ng/mL）	膏霜		水剂
编号	物质名称	添加水平/（ng/mL）	回收率/%	RSD/%	回收率/%	RSD/%
1	曲吡那敏	0.48	99.6	3.3	103.2	3.2
		2.41	101.0	2.2	99.3	1.9
		7.71	98.9	1.4	105.1	0.3
2	阿司咪唑	0.55	95.9	3.6	103.8	6.0
		2.77	97.1	2.7	104.9	3.4
		8.87	93.7	3.3	103.2	1.7
3	赛庚啶	0.56	98.4	6.2	104.0	5.1
		2.81	99.6	5.7	103.9	2.0
		9.00	98.7	0.4	100.7	3.0
4	氯丙嗪	0.55	101.6	2.5	105.7	5.0
		2.75	100.6	2.4	104.6	1.8
		8.81	99.2	1.5	102.5	0.7
5	特非那定	0.52	101.3	3.3	107.2	4.1
		2.60	101.7	2.8	109.0	2.8
		8.32	104.7	1.0	111.2	2.5
6	司他斯汀	0.71	99.4	3.2	100.8	4.4
		3.57	100.5	2.7	100.4	1.4
		11.43	100.0	1.4	101.4	0.4
7	西咪替丁	0.51	105.1	5.1	106.2	5.1
		2.57	100.8	2.2	100.3	3.2
		8.23	102.8	2.2	102.6	2.6
8	二氧丙嗪	0.49	112.8	7.0	108.2	7.3
		2.47	100.3	5.4	102.5	3.6
		7.92	103.3	4.0	99.6	3.4
9	氯苯那敏	0.56	102.2	1.9	102.2	3.3
		2.78	97.7	1.5	107.3	2.0
		8.90	101.2	1.8	101.4	1.9
10	羟嗪	0.59	101.4	3.8	105.6	5.2
		2.93	102.2	2.8	109.7	1.4
		9.36	99.2	2.3	105.4	2.6
11	奋乃静	0.47	101.2	0.9	103.2	3.0
		2.36	99.0	1.6	105.1	2.6
		7.55	98.9	0.9	104.1	1.6
12	氯苯沙明	0.49	110.4	14.8	115.9	12.0
		2.47	105.6	13.7	111.4	11.1
		7.91	104.6	7.0	101.3	0.9
13	奥洛他定	0.49	98.9	3.5	103.2	9.1
		2.47	100.7	2.7	102.8	3.4
		7.90	96.7	2.1	99.1	3.1
14	多西拉敏	0.49	100.5	2.4	105.2	4.2
		2.45	99.4	2.1	101.2	1.0
		7.84	95.0	2.0	100.9	0.3
15	苯海拉明	0.57	96.7	4.3	105.6	3.3
		2.86	99.8	3.8	103.7	3.3
		9.17	106.4	2.3	104.5	1.4
16	氯雷他定	0.54	104.6	5.4	101.5	1.6
		2.72	101.5	3.3	103.0	1.5
		8.70	100.5	3.1	103.0	0.8
17	依匹斯汀	0.66	105.3	6.1	99.0	4.6
		3.28	100.2	2.3	99.9	2.4
		10.50	95.4	2.7	106.5	2.8
18	非索非那定	0.58	101.0	3.8	104.8	7.1
		2.88	97.6	3.8	99.1	4.7
		9.22	96.7	3.4	102.5	3.3
19	美沙吡林	0.49	102.0	3.2	106.0	2.7
		2.46	104.9	1.0	100.7	1.1
		7.87	94.0	0.9	101.3	1.0
20	赛克利嗪	0.54	97.5	3.3	99.0	3.2
		2.72	103.4	3.2	100.5	1.6
		8.70	96.0	1.4	105.3	0.8
21	卢帕他定	0.50	107.4	3.0	112.6	3.3
		2.51	99.7	2.2	102.3	3.7
		8.04	101.5	1.2	102.0	2.8
22	氟奋乃静	0.51	106.6	2.4	109.6	3.6
		2.57	97.7	2.0	101.8	1.1
		8.21	101.4	1.8	102.3	0.8
23	西替利嗪	0.67	98.9	3.1	96.4	6.2
		3.36	100.3	0.7	101.2	3.3
		10.76	100.4	1.1	107.5	2.4
24	酮替芬	0.58	103.8	5.2	104.7	4.7
		2.88	101.0	2.9	102.3	4.1
		9.23	99.9	1.5	99.3	4.0
25	溴苯那敏	0.56	100.5	2.8	102.9	3.9
		2.79	102.7	1.5	104.7	2.6
		8.91	102.5	1.4	104.2	2.0
26	地氯雷他定	0.51	80.9	10.7	90.2	10.0
		2.53	82.2	9.0	103.1	4.5
		8.10	81.6	7.7	94.9	2.4
27	二苯拉林	0.50	106.2	1.5	100.8	5.2
		2.50	99.5	2.1	101.5	1.9
		8.00	99.0	2.1	100.8	0.5
28	赛庚啶杂质1	0.44	96.2	6.5	102.6	3.4
		2.18	95.1	4.2	109.9	3.1
		6.96	94.7	0.5	106.1	3.8
29	异丙嗪	0.54	98.0	4.2	99.0	2.7
		2.70	101.3	2.2	104.9	2.3
		8.63	99.5	1.5	100.5	2.6

Tab. 4

References 12

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编号	物质名称	母离子m/z	子离子m/z	CE/V	DP/V
1	曲吡那敏	256.2	211.1 91.1	20 40	35
2	阿司咪唑	459.2	218.2 135.2	35 45	130
3	赛庚啶	288.1	191.1 96.2	37 32	90
4	氯丙嗪	319.1	86.1 58.1	25 67	55
5	特非那定	472.6	436.5 454.4	35 29	80
6	司他斯汀	358.2	215.0 144.2	20 14	25
7	西咪替丁	253.0	159.1 117.2	19 21	30
8	二氧丙嗪	317.1	86.2 272.2	28 28	50
9	氯苯那敏	275.0	230.1 167.0	20 52	30
10	羟嗪	375.1	201.1 166.1	24 55	45
11	奋乃静	404.2	171.3 143.1	32 39	50
12	氯苯沙明	304.2	215.0 180.0	16 39	30
13	奥洛他定	338.1	247.2 165.1	32 33	75
14	多西拉敏	271.1	182.1 167.1	20 45	30
15	苯海拉明	256.1	167.1 152.0	14 47	10
16	氯雷他定	383.1	337.1 267.2	31 45	70
17	依匹斯汀	250.1	193.2 131.2	46 43	120
18	非索非那定	502.3	171.1 466.4	50 38	110
19	美沙吡林	262.1	217.1 97.0	18 33	30
20	赛克利嗪	267.1	167.2 152.1	17 53	20
21	卢帕他定	416.2	309.2 282.2	25 30	150
22	氟奋乃静	438.2	171.2 143.2	35 40	70
23	西替利嗪	389.2	201.1 166.2	23 55	40
24	酮替芬	310.1	96.1 213.0	30 38	125
25	溴苯那敏	319.0	274.1 167.1	22 55	30
26	地氯雷他定	311.1	259.1 294.1	28 25	110
27	二苯拉林	282.1	167.2 152.1	19 57	35
28	赛庚啶杂质1	306.2	191.1 288.2	42 22	75
29	异丙嗪	285.1	86.0 198.2	20 27	20

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[15]	Feng Liu, Yuanchang Deng, Guohong Ying, Xiaowei Wang. Establishment of duplex-PCR method for rapid detection of Pluralibacter gergoviae [J]. China Surfactant Detergent & Cosmetics, 2024, 54(1): 45-50.

Determination of 29 anti-allergy drugs by UPLC-MS/MS in cosmetics

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