超高效液相色谱-四级杆/飞行时间高分辨质谱法测定膏霜类化妆品中的阿托品

doi:10.3969/j.issn.2097-2806.2023.06.013

Abstract

Abstract:

A quick method for detecting atropine in cream cosmetics was devised using ultra performance liquid chromatography-quadrupole/time-of-flight high-resolution mass spectrometry （UPLC-QTOF-MS/MS）, and a different approach was created for establishing an atropine database. The samples were ultrasonically extracted with 80% （V/V） acetonitrile solution. After centrifugation, the extracts were separated and filtered. The separation was performed on an ACQUITY UPLC^® BEH C₁₈ （2.1 mm×100 mm, 1.7 μm） column in electrospray positive ionization mode with MSE mode for characterization, multiple reaction monitoring （MRM） mode for data acquisition and quantification by external standard method of matrix solvent standard solution. The atropine shows a good linearity （R²>0.999 0） in the range of 3.0-100.0 ng/mL. The limit of detection （LOD） of the method is 1.0 ng/mL and the limit of quantification （LOQ） is 3.0 ng/mL. The average recoveries of atropine are 107.9%, 97.0% and 105.3% at the spiked levels of 20, 50 and 80 ng/mL, respectively. The RSDs are 4.2%, 3.0% and 3.2%, respectively （n=6）. This method is simple, sensitive and suitable for the rapid screening and quantitative analysis of atropine in cosmetics.

Key words: ultra performance liquid chromatography-quadrupole/time-of-flight high-resolution mass spectrometry （UPLC-QTOF-MS/MS）, alkaloids, atropine, cream cosmetic

CLC Number:

TQ658

Qiu Qianqian, Lu Yong, Wang Xinran, Wu Baojin, Wang Haiyan, Sun Jianbo. Determination of atropine in cream cosmetics by ultra performance liquid chromatography-quadrupole/time-of-flight high-resolution mass spectrometry[J].China Surfactant Detergent & Cosmetics, 2023, 53(6): 706-713.

Figures/Tables 10

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References 13

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Compound	Precursor ion, m/z	Product ion, m/z	Sampling cone/V	CE ^a/eV
Atropine	290.2	93.1	20.0	24.0
Atropine	290.2	124.2 ^b	20.0	24.0

Compound	Formula	Neutral mass/Da	Precursor ion/（m/z）	Mass error/mDa	Retention time/min	Product ion/（m/z）
Compound	Formula	Neutral mass/Da	Precursor ion/（m/z）	Mass error/mDa	Retention time/min	F₁	F₂	F₃
Atropine	C₁₇H₂₃NO₃	289.4	290.2	0.9	3.5	133.1	89.1	86.1

Level	Test count	Spiked/（ng/mL）	Recoveries/%	Average recoveries/%	RSD/%
L^a	1.0	20.0	111.7	107.9	4.2
	2.0	20.0	99.2
	3.0	20.0	107.2
	4.0	20.0	108.8
	5.0	20.0	109.6
	6.0	20.0	110.6
M^b	1.0	50.0	95.4	97.0	3.0
	2.0	50.0	99.2
	3.0	50.0	92.7
	4.0	50.0	99.2
	5.0	50.0	100.0
	6.0	50.0	95.2
H^c	1.0	80.0	99.7	105.3	3.2
	2.0	80.0	105.6
	3.0	80.0	103.1
	4.0	80.0	108.5
	5.0	80.0	108.5
	6.0	80.0	106.6

Inspection materials	Target	RSD/%
Inspection materials	Target	20 ng/mL	50 ng/mL	80 ng/mL
Blank substrate addition	Atropine	3.5	3.9	4.5

Inspection materials	Target	RSD/%
Inspection materials	Target	20 ng/mL	50 ng/mL	80 ng/mL
Blank substrate addition	Atropine	4.8	3.6	3.8

Determination of atropine in cream cosmetics by ultra performance liquid chromatography-quadrupole/time-of-flight high-resolution mass spectrometry

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Inspection materials	Target	RSD/%
Inspection materials	Target	Daytime	Intraday
Blank substrate addition	Atropine	3.8	4.0

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