首页|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

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

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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)>0.9990,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.
Determination of atropine in cream cosmetics by ultra performance liquid chromatography-quadrupole/time-of-flight high-resolution mass spectrometry
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>0.9990)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.

ultra performance liquid chromatography-quadrupole/time-of-flight high-resolution mass spectrometry(UPLC-QTOF-MS/MS)alkaloidsatropinecream cosmetic

邱倩倩、路勇、王欣然、吴宝金、王海燕、孙建博

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中国药科大学,江苏 南京 210009

中国食品药品检定研究院 国家药品监督管理局化妆品研究与评价重点实验室,北京 100050

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

国家科技重大专项

2022FY101202

2023

日用化学工业(中英文)
中国日用化学工业研究院

日用化学工业(中英文)

CSTPCD北大核心
影响因子:0.553
ISSN:1001-1803
年,卷(期):2023.53(6)
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