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首页|期刊导航|分析测试学报|超高效液相色谱-四极杆-飞行时间高分辨质谱用于化妆品中15种前列腺素类似物的快速筛查和测定

超高效液相色谱-四极杆-飞行时间高分辨质谱用于化妆品中15种前列腺素类似物的快速筛查和测定OA北大核心CSTPCD

Rapid Screening and Determination of 15 Prostaglandin Analogues in Cosmetics by Ultra Performance Liquid Chromatography-Quadru-pole-Time-of-flight High-resolution Mass Spectrometry

中文摘要英文摘要

建立了超高效液相色谱-四极杆-飞行时间高分辨质谱(UPLC-Q-TOF MS)快速筛查和测定化妆品中15种前列腺素类似物的方法.样品以饱和氯化钠作为分散剂(蜡质类样品以四氢呋喃分散),经乙腈提取,离心取上清液过滤后,采用Poroshell 120 EC-C18柱(150 mm×3.0 mm,2.7 μm)分离,以5 mmol/L甲酸铵(含0.1%甲酸)-乙腈为流动相梯度洗脱.在ESI正离子模式下,采用Targeted MS/MS模式采集15种前列腺素类似物的质谱信息,构建筛查数据库进行快速筛查,确证后的目标物通过外标法定量.结果表明,15种前列腺素类似物的线性关系良好,相关系数(r2)均大于0.99;检出限为0.3~17.6 μg/g,定量下限为1.1~58.8 μg/g.在低、中、高3个加标水平下,水剂、膏霜、乳类、粉类、凝胶5类化妆品基质的回收率为70.1%~134%,相对标准偏差不大于7.5%.该方法简单高效、准确度好,可用于化妆品中前列腺素类似物的定性确证和定量分析,为化妆品风险识别提供技术支撑.

In this study,an ultra performance liquid chromatography-quadrupole-time-of-flight high-resolution mass spectrometry(UPLC-Q-TOF MS)method was developed for the rapid screening and quantitative analysis of 15 prostaglandin analogues in cosmetics.The analytes in sample were dis-persed in saturated sodium chloride solution(wax samples were dispersed with tetrahydrofuran),then extracted with acetonitrile.After centrifugation and filtration,the UPLC separation of 15 prosta-glandin analogues was performed on Poroshell 120 EC-C18 column(150 mm×3.0 mm,2.7 μm),us-ing 5 mmol/L ammonium formate(containing 0.1%formic acid)solution and acetonitrile as mobile phase by gradient elution.15 prostaglandin analogues were detected by positive ion electrospray ion-ization(ESI)in the Targeted MS/MS mode.To construct a screening library with the software by the retention time,exact mass of primary parent ions,isotope abundance ratio and secondary sub-ion li-brary matching were collected.The results of matching were used to rapid identification of 15 prosta-glandin analogues in cosmetics.The quantification of primary parent ions was performed by external standard method.15 prostaglandin analogues were all well separated.The linear correlation coeffi-cients(r2)were more than 0.99.The limits of detection(LODs)ranged of 0.3-17.6 μg/g and the lim-its of quantitation(LOQs)ranged of 1.1-58.8 μg/g.The recoveries at three spiked levels in lotion,cream,emulsion,powder and gel matrices varied from 70.1%to 134%,with relative standard devi-ations not more than 7.5%.The established method is rapid,simple and accurate,which is suitable for the screening and determination of 15 prostaglandin analogues in cosmetics,providing technical support for cosmetic risk identification.

陈安丽;张静;黄子沣;严小红

广州市药品检验所,广东 广州 510160

化学

超高效液相色谱-四极杆-飞行时间高分辨质谱快速筛查化妆品前列腺素类似物

ultra performance liquid chromatography-quadrupole-time-of-flight high-resolution mass spectrometryrapid screeningcosmeticsprostaglandin analogues

《分析测试学报》 2024 (007)

1011-1017 / 7

广州市市场监督管理局科技项目(2022kj28)

10.12452/j.fxcsxb.24033102

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