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

摘要/Abstract

摘要：

建立了超声辅助提取-超高效液相色谱-四级杆/飞行时间高分辨质谱快速测定膏霜类化妆品中阿托品的分析方法和阿托品数据库。样品经80%乙腈溶液超声提取，离心后过滤。经ACQUITY UPLC^® BEH C₁₈ （2.1 mm×100 mm，1.7 μm）色谱柱分离，在电喷雾正离子模式下，采用MSE模式对其进行定性，采用多反应监测（MRM）模式进行数据采集，基质溶剂标准溶液外标法定量。结果显示，阿托品在3.0~100.0 ng/mL的质量浓度范围内线性关系良好，相关系数（R²）>0.999 0，方法的检出限为1.0 ng/mL，定量限为3.0 ng/mL。在质量浓度分别为20，50，80 ng/mL的加标水平下，阿托品的平均回收率分别为107.9%，97.0%，105.3%。RSD分别为4.2%，3.0%，3.2%（n=6）。该方法操作简单，灵敏度高，适用于膏霜类化妆品中阿托品的快速筛查和定量分析。

关键词: 超高效液相色谱-四极杆/飞行时间高分辨质谱法, 生物碱, 阿托品, 膏霜类化妆品

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

中图分类号:

TQ658

邱倩倩, 路勇, 王欣然, 吴宝金, 王海燕, 孙建博. 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[J]. 日用化学工业（中英文）, 2023, 53(6): 706-713.

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.

图/表 10

参考文献 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