UPLC-MS/MS测定化妆品中15种禁用物质

doi:10.3969/j.issn.1001-1803.2020.01.012

Abstract

Abstract:

An analytical method of ultra performance liquid chromatography-triple quadrupole mass spectrometry （UPLC-MS/MS） was developed for the simultaneous determination of 15 prohibited substances （diphenhydramine, tripelennamine, chlorpheniramine, etc.） in cosmetics. The UPLC separation was carried out on a Waters Acquity UPLC? BEH C₁₈ column （1.7 μm × 2.1 mm × 50 mm） by gradient elution using methanol and ammonium acetate-formic acid solution. The flow rate was 0.4 mL/min and the sample injection amount was 3 μL. The electrospray ionization source in positive ion mode （ESI ⁺） was used for qualitative analysis and quantitative analysis of fifteen prohibited drugs in the multiple reaction monitoring （MRM） mode. The established method exhibited a good linear relationship in the corresponding concentration range. The linear correlation coefficient is 0.999 3-0.999 9; the recoveries of standard addition are between 87.21%-99.39% （n=3）; the relative standard deviation is 2.28%-5.27% （n=6）; the detection limit range is 0.014 3-0.239 2 mg/kg; the limit of quantification range is 0.004 3-0.797 2 mg/kg. The method is accurate and reliable, and is suitable for simultaneous determination of various prohibited substances in cosmetics.

Key words: prohibited substance, cosmetics, ultra performance liquid chromatography-triple quadrupole mass spectrometry

CLC Number:

TQ658

CAO Hai-rong,LI Xiao-yu,XUE Xiao-kang. Determination of fifteen prohibited substances in cosmetics by ultra performance liquid chromatography-triple quadrupole mass spectrometry[J].China Surfactant Detergent & Cosmetics, 2020, 50(1): 64-70.

Figures/Tables 8

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References 16

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组分名称	母离子（m/z）	子离子（m/z）	锥孔电压/V	子离子的碰撞气能量/V
盐酸苯海拉明	256.2	167.1	26	12
盐酸曲吡那敏	256.2	211.1	26	14
马来酸氯苯那敏	275.1	230.1	34	15
盐酸异丙嗪	285.1	86.2	34	18
盐酸赛庚啶	288.2	96.2	34	28
地氯雷他定	311.1	259.1	35	24
盐酸氯丙嗪	319.1	86.2	34	21
马来酸溴苯那敏	319.1	274.0	34	18
盐酸羟嗪	375.2	201.0	34	19
氯雷他定	383.1	337.0	34	22
盐酸西替利嗪	389.1	201.0	34	20
奋乃静	404.2	171.1	34	24
盐酸氟奋乃静	438.2	143.1	34	30
阿司咪唑	459.3	135.1	34	35
特非那定	472.3	436.3	40	26

组分名称	线性范围/ （μg·L^-1）	回归方程	r	检出限/（mg·kg^-1）	定量限/（mg·kg^-1）
盐酸苯海拉明	5~100	y = 5 296.8x - 3 586.1	0.999 0	0.007 9	0.026 2
盐酸曲吡那敏	5~100	y = 8 508.2x -7 771.3	0.999 9	0.023 0	0.076 7
马来酸氯苯那敏	5~100	y = 3 593.8x -2 925.0	0.999 8	0.037 6	0.125 3
盐酸异丙嗪	5~100	y = 4 596.2x - 1 266.2	0.999 9	0.011 4	0.038 0
盐酸赛庚啶	5~100	y = 1 305.8x - 434.0	0.999 9	0.039 5	0.131 6
地氯雷他定	5~100	y = 306.6x - 225.1	0.999 8	0.061 7	0.205 6
盐酸氯丙嗪	5~100	y = 4 250.4x - 968.8	0.999 9	0.018 5	0.061 6
马来酸溴苯那敏	5~100	y = 2 290.4x - 6 689.9	0.999 6	0.239 2	0.797 2
盐酸羟嗪	5~100	y = 2 700.4x + 9 165.1	0.999 9	0.084 4	0.281 5
氯雷他定	5~100	y = 908.5x + 155.2	0.999 9	0.004 3	0.014 3
盐酸西替利嗪	5~100	y = 741.8x + 205.2	0.999 3	0.084 9	0.282 9
奋乃静	5~100	y = 851.0x + 73.6	0.999 9	0.032 5	0.108 2
盐酸氟奋乃静	5~100	y = 621.2x + 2.8	0.999 9	0.004 5	0.015 1
阿司咪唑	5~100	y = 2 057.3x - 1 029.6	0.999 8	0.054 2	0.180 7
特非那定	5~100	y = 1 134.2x + 1 957.1	0.999 9	0.010 1	0.033 7

组分名称	ρ（添加）/（μg·L^-1）	ρ（实际）/（μg·L^-1）	加标回收率/%	平均加标回收率/%	组分名称	ρ（添加）/（μg·L^-1）	ρ（实际）/（μg·L^-1）	加标回收率/%	平均加标回收率/%
盐酸苯海拉明	41.39	36.73	88.74	94.15	盐酸曲吡那敏	45.25	40.40	89.27	93.05
	62.08	58.32	93.93			67.88	62.25	91.71
	82.78	82.59	99.78			90.51	88.86	98.18
马来酸氯苯那敏	41.41	34.25	82.71	89.24	盐酸异丙嗪	42.25	39.13	92.62	99.39
	62.12	55.53	89.39			63.38	63.01	99.41
	82.83	79.20	95.63			84.51	89.70	106.15
盐酸赛庚啶	42.37	37.20	87.79	93.58	地氯雷他定	39.98	34.58	86.47	92.70
	63.55	58.81	92.54			59.98	56.01	93.39
	84.74	85.09	100.41			79.97	78.55	98.22
盐酸氯丙嗪	40.59	34.91	86.03	89.84	马来酸溴苯那敏	42.50	35.77	84.16	90.40
	60.88	54.78	89.98			63.76	56.41	88.48
	81.17	75.91	93.52			85.01	83.78	98.56
盐酸羟嗪	41.90	35.40	84.49	89.96	氯雷他定	40.45	35.63	88.08	93.55
	62.86	54.16	86.17			60.68	56.52	93.14
	83.81	83.16	99.23			80.91	80.44	99.42
盐酸西替利嗪	39.87	34.44	86.39	91.40	奋乃静	42.22	35.46	83.99	87.66
	59.80	53.71	89.81			63.33	55.34	87.39
	79.73	78.15	98.01			84.44	77.33	91.58
盐酸氟奋乃静	40.06	35.08	87.57	92.76	阿司咪唑	36.81	29.75	80.82	87.21
	60.09	55.35	92.10			55.21	47.74	86.46
	80.12	79.00	98.59			73.62	69.45	94.34
特非那定	40.14	35.04	87.30	92.83
	60.21	55.42	92.05
	80.28	79.59	99.14

组分名称	ρ（添加）/（μg·L^-1）	精密度/%	平均精密度/%	组分名称	ρ（添加）/（μg·L^-1）	精密度/%	平均精密度/%
盐酸苯海拉明	40	8.46	3.97	盐酸曲吡那敏	40	7.10	5.27
	60	2.33			60	5.66
	80	1.13			80	3.06
马来酸氯苯那敏	40	6.23	5.16	盐酸异丙嗪	40	5.03	2.87
	60	3.65			60	2.17
	80	5.59			80	1.42
盐酸赛庚啶	40	4.91	3.06	地氯雷他定	40	6.71	3.45
	60	2.34			60	2.26
	80	1.94			80	1.38
盐酸氯丙嗪	40	4.49	2.80	马来酸溴苯那敏	40	3.96	4.03
	60	1.97			60	3.65
	80	1.95			80	4.48
盐酸羟嗪	40	5.85	2.92	氯雷他定	40	3.32	2.82
	60	2.03			60	2.34
	80	0.87			80	2.79
盐酸西替利嗪	40	6.60	3.52	奋乃静	40	7.42	4.24
	60	2.47			60	2.93
	80	1.49			80	2.37
盐酸氟奋乃静	40	6.48	3.65	阿司咪唑	40	5.03	3.53
	60	2.08			60	3.15
	80	2.40			80	2.42
特非那定	40	3.14	2.28
	60	1.64
	80	2.05

Determination of fifteen prohibited substances in cosmetics by ultra performance liquid chromatography-triple quadrupole mass spectrometry

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t/min	φ/%
t/min	甲醇	乙酸铵-甲酸水溶液
0	40	60
1.0	40	60
2.0	50	50
4.0	50	50
5.0	65	35
9.0	100	0
11.0	100	0
12.0	40	60
15.0	40	60

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